CN2227338Y - Liquid chromatography device for separating dead oil component - Google Patents
Liquid chromatography device for separating dead oil component Download PDFInfo
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- CN2227338Y CN2227338Y CN 95206455 CN95206455U CN2227338Y CN 2227338 Y CN2227338 Y CN 2227338Y CN 95206455 CN95206455 CN 95206455 CN 95206455 U CN95206455 U CN 95206455U CN 2227338 Y CN2227338 Y CN 2227338Y
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Abstract
The utility model relates to a liquid chromatography device for separating dead oil component. The utility model is mainly composed of a chromatographic column (1, 2), a detector (D), a six-way change-over valve (3, 4, 5), a six-way sampling valve (6), a chromatographic pump (p), connecting pipes (10-20), and other components. The utility model is characterized in that a double chromatographic column system composed of a gelatinous retention chromatography column (1) and a separation chromatographic column (2) are adopted; three six-way change-over valves which can change the flow path of the chromatographic column are arranged between the two chromatographic columns; meanwhile, a moving wire detector is adopted as the detector after chromatographic separation. When the liquid chromatography device is used, the contents of the saturated hydrocarbon, the arene, and the colloid in petroleum heavy oil or residual oil can be separated and analysed within 15 minutes.
Description
The utility model is about separating the liquid-chromatography apparatus of heavy oil hydrocarbon system component, belonging to the technical field that chromatographic resolution is analyzed.
The black petroleum products component analysis, it is one of common analysis project of heavy oil upgrading, past classical adsorption chromatography device commonly used carries out (volume such as Yang Cuiding, " petrochemical complex analytical approach ", Science Press, 1990, the 31-33 page or leaf), when adopting this device to analyze, the first process of sample normal heptane is settled out bituminous matter, after inciting somebody to action deasphalting partly is separated into stable hydrocarbon, aromatic hydrocarbons and colloid with the alumina adsorption chromatographic column.Owing to each separate employed heavy oil sample size and reach the 1-2 gram, be with a large amount of solvent washings, not only take a lot of trouble during operating cost, but also will reach analysis time about 1 week through the repeatedly evaporation of solvent and the constant weight of sample.The poor repeatability of measuring, common highly effective liquid phase chromatographic device are one of desirable means of present hydrocarbon system separation.But because the classification of crude oil is various, heavy oil is formed complicated, polarity thing content height, and the K value of each hydrocarbon system multiple reason such as wide that distributes also is difficult to the baseline separation of each hydrocarbon system's component on liquid chromatography(LC in single chromatographic column or the single elution requirement realization heavy oil.People such as Elsa lundance propose to use column switching technique and use ultraviolet and differential refraction detector detects, can address this problem effectively (Liq.chromatogr.8[6], 1035,1985), yet, rising along with the analytic sample boiling point, when using this device to analyze, the baseline separation of stable hydrocarbon and aromatic hydrocarbons is tending towards difficulty, the adsorption column that requires to use must have very high activity, in use, also can equate the influence of factor owing to being subjected to flowing, the active of adsorption column constantly descends, and can not guarantee the baseline separation between each hydrocarbon system of heavy oil, owing to use ultraviolet and differential refraction detector to detect, also must often carry out the mensuration of cumbersome quantitative correction factor simultaneously.Therefore, this device can not be as the control device of conventional heavy oil alkyl analysis.
The purpose of this utility model is the deficiency at prior art, provide a kind of can be efficiently fast the compartment analysis initial boiling point greater than the liquid-chromatography apparatus of stable hydrocarbon, aromatic hydrocarbons and gum level in 200 ℃ the heavy oil component.
The utility model is realized by following proposal: this liquid-chromatography apparatus mainly is made up of parts such as chromatographic column, detecting device, six-way injection valve, six direction changeover valves, chromatogram pump, connecting pipes, it is characterized in that adopting the double-colored spectrum column system of forming by colloid reservation chromatographic column and separation chromatography post, between two chromatographic columns, be provided with three six direction changeover valves that can change the chromatographic column stream, simultaneously, the detecting device after using moving wire detector as chromatographic resolution.Use this liquid-chromatography apparatus can be in 15 minutes the content of stable hydrocarbon, aromatic hydrocarbons and colloid in compartment analysis black petroleum products or the residual oil.
Describing structure of the present utility model in detail below by accompanying drawing forms.
Fig. 1 is a structural representation of the present utility model.Among Fig. 1: 1 for colloid keeps chromatographic column, and 2 is the separation chromatography post, and 3,4,5 is six direction changeover valves, 6 is six-way injection valve, and 7 is the chromatographic column activation box, and 8 is system's housing, 9 is insulation material, and 10～20 is connecting pipe, and 21～24 is the interface at chromatographic column (1,2) two ends.
As shown in Figure 1: there is a rectangle chromatographic column activation box (7) that is complementary with its size the outside of separation chromatography post (2), the inwall of activation box (7) is lined with insulation material (9), with chromatographic column (2) up and down the connecting pipe (15,14) that links to each other respectively of two end interfaces (23, the 24) top layer that passes activation box (7) and insulation material (9) link to each other with six direction changeover valves (5) with bottom; Colloid chromatographic column (1) two end interfaces (21,22) up and down links to each other with six direction changeover valves (3) by connecting pipe (11,16) respectively; Connect by connecting pipe (12,13,17) respectively between six direction changeover valves (3,4,5); Six direction changeover valves (3) are connected with six-way injection valve (6) by connecting pipe (10); Six-way injection valve (6) links to each other with chromatogram pump (P) by connecting pipe (19); Six direction changeover valves (3) link to each other with moving wire detector (D) by connecting pipe (18); Six direction changeover valves (5) are connected with nitrogen cylinder by connecting pipe (20).
Fig. 2 is the structural representation of end interface (22) under the chromatographic column (1).
As shown in Figure 2: earlier nut (22-3), sword ring (22-2) are enclosed within on the connecting pipe (16), then connecting pipe (16) is inserted in the chromatographic column termination (22-1), load onto sword ring (22-2), use nut (22-3) to tighten at last, end interface (22) under the chromatographic column (1) can be connected with connecting pipe (16) like this.Chromatographic column (1) goes up end interface (21), chromatographic column (2) the same interface of reason (22) that is connected with connecting pipe of two end interfaces (23,24) up and down.
It is the stainless steel chromatogram post of column length 30-50mm, internal diameter 4-4.6mm that the said colloid of the utility model keeps chromatographic column (1), is filled with the cyano group bonded stationary phase of 5-10 micron in the post; Said separation chromatography post (2) is about column length 300mm, the stainless steel chromatogram post of internal diameter 4-10mm, is filled with any stationary phase that is selected from silica gel, aluminium oxide, the silica gel-aluminium oxide in the post, granularity 5-40 micron; Said six direction changeover valves (3,4,5) are Rheodyne7000 series transfer valve, and about withstand voltage 34MPa, caliber interface and external diameter are that the stainless-steel tube about 1/16 inch is complementary; Said six-way injection valve (6) is the Rheodyne7125 type valves, and the stainless steel connecting pipe that its caliber interface and external diameter are 1/16 inch is complementary.
The said chromatographic column activation box of the utility model (7) is a metal material, a hair dryer is housed as thermal source at the bottom of the case, and the thermopair detected temperatures is housed in the casing, by the heating of temperature controller control hair dryer; Said system housing (8) is a metal material; Said insulation material (9) is selected from insulation materials such as asbestos cloth or sheet asbestos.
The said connecting pipe of the utility model (10～20) is the stainless-steel tube of about 1/16 inch of external diameter.
The said moving wire detector of the utility model (D) is the disclosed a kind of hydrocarbon type test high performance liquid chromatography moving wire detector of CN93216473.0.
When being used to analyze, the utility model carries out according to following steps:
1. at first use the hexane rinse-system, moving phase (hexane) is sent by chromatogram pump (P), through six-way injection valve (6), connecting pipe (10), six direction changeover valves (3), connecting pipe (11) enters chromatographic column (1), after moving phase is come out from chromatographic column (1) through connecting pipe (16), six direction changeover valves (3), connecting pipe (12), six direction changeover valves (4), connecting pipe (13), enter chromatographic column (2) behind six direction changeover valves (5) and the connecting pipe (14), pass through connecting pipe (15) again from the moving phase that chromatographic column (2) is come out, six direction changeover valves (5), connecting pipe (17), six direction changeover valves (3) and connecting pipe (18) enter moving wire detector (D).
2. after device to be detected (D) conditional stability, annotate 1-2 microlitre oil sample by six-way injection valve (6), carry down at the moving phase hexane, oil sample is through parts 10,3,11 enter chromatographic column (1), colloid in the oil sample partly is retained on the chromatographic column (1), and stable hydrocarbon in the oil sample and aromatic hydrocarbons part are left chromatographic column (1) with the moving phase hexane, through parts 16,3,12,4,13,5 and parts 14 after enter chromatographic column (2), rotate six logical switchings this moment and dodge (3), make chromatographic column (1) be isolated out from stream, moving phase is through parts 6,10,3,12,4,13,5 and parts 14 enter chromatographic column (2).
3. the stable hydrocarbon of sample and aromatic hydrocarbons obtain baseline separation by chromatographic column (2), send into behind the stable hydrocarbon flow path parts 15,5,17,3,18 in the detecting device (D) and detect, after stable hydrocarbon flows out, change the moving phase hexane into methylene chloride, the latter elutes aromatic hydrocarbons from chromatographic column (2), send into detecting device (D).
4. rotate six direction changeover valves (4,5) then, chromatographic column (2) is isolated out from stream, the mobile phase dichloromethane parts 6,10,3,12,4,13,5,17,3,16 of flowing through enter chromatographic column (1), and the colloid on it is eluted, and send into detecting device D behind parts 11,3,18.
5. rotate six direction changeover valves (3,4,5), stream is returned to initial state, do the separation of next sample and prepare.
The utlity model has following advantage:
1. owing to used double-colored spectrum column system, thereby can utilize column switching technique and gradient solvent program successfully heavy oil to be separated into stable hydrocarbon fast, aromatic hydrocarbons and colloid are applicable to that initial boiling point greater than any petroleum fraction of 200 ℃, comprises vacuum residuum.
2. owing to be used, can realize heavy oil hydrocarbon type test high efficiency, can finish the analysis of 1 heavy oil sample in 15 minutes, and classical chromatogram arrangement analysis time is about 1 week that common liquid-chromatography apparatus separates and needs a few hours with moving wire detector.
(3) the utility model is owing to using column switching technique, avoided colloid to enter the irreversible adsorption phenomenon that is caused in the chromatographic column (2) that is filled with silica gel.In addition,, can change the stream of chromatographic column, avoid blowback operation, can improve the serviceable life of chromatographic column (2) so greatly chromatographic column (2) owing between two chromatographic columns three six direction changeover valves have been installed.
(4) the utility model has the fast activating function to chromatographic column (2) owing in the outside of chromatographic column (2) chromatographic column activation box (7) is housed, and has guaranteed chromatographic column (2)) to the required activity of separating between the stable hydrocarbon of heavy oil and aromatic hydrocarbons.Because the activation furnace heating is by the heating of temperature controller control hair dryer, therefore has and heat up and the fast characteristics of cooling rate in addition.
The following examples will the utility model is described in further detail.
Example
The utility model chromatographic column (1) is selected the stainless steel column of long 30mm, internal diameter 4mm for use, is filled with the cyano group bonded stationary phase of 5-10 micron in the post.Chromatographic column (2) is selected the stainless steel column of long 300mm, internal diameter 10mm for use, is filled with the silica gel of 5-40 micron in the post.It is 1/16 inch stainless-steel tube that connecting pipe (10～20) is selected external diameter for use.Use the long residuum of this liquid-chromatography apparatus compartment analysis＞350 ℃.
The chromatogram that Fig. 3 obtains when being used for the long residuum of compartment analysis＞350 ℃ for the utility model.S is that stable hydrocarbon, A are that aromatic hydrocarbons, R are colloid among Fig. 3.
As seen from Figure 3: when the utility model is used for analyzing＞350 ℃ long residuum, only just can obtain very desirable SAR chromatogram (Fig. 3) with about 10 minutes, and need a few hours when separating heavy oil with common liquid-chromatography apparatus, it can be said that brightly, the utlity model has efficient, characteristics of stable hydrocarbon, aromatic hydrocarbons and gum level in the compartment analysis heavy oil fast.
Claims (6)
1. the liquid-chromatography apparatus of a compartment analysis heavy oil component, comprise six-way injection valve (6), chromatogram pump (P), connecting pipe parts such as (10～20), it is characterized in that chromatographic column is a dual column system, form by colloid reservation chromatographic column (1) and separation chromatography post (2), between two chromatographic columns, three six direction changeover valves (3 that can change the chromatographic column stream are housed, 4,5), detecting device (D) after using moving wire detector as chromatographic resolution, its structure is: there is a rectangular chromatographic column activation box (7) that is complementary with its size the outside of separation chromatography post (2), the inwall of activation box (7) is lined with insulation material (9), with chromatographic column (2) two end interfaces (23 up and down, 24) connecting pipe (15 that links to each other respectively, 14) top layer that passes activation box (7) and insulation material (9) links to each other with six direction changeover valves (5) with bottom, chromatographic column (1) is two end interfaces (21 up and down, 22) respectively by connecting pipe (11,16) link to each other with six direction changeover valves (3), six direction changeover valves (3,4,5) pass through connecting pipe (12 between respectively, 13,17) connect, six direction changeover valves (3) are connected with six-way injection valve (6) by connecting pipe (10), six-way injection valve (6) links to each other with chromatogram pump (P) by connecting pipe (19), six direction changeover valves (3) link to each other with detecting device (D) by connecting pipe (18), and six direction changeover valves (5) link to each other with nitrogen cylinder by connecting pipe (20).
2. according to the said liquid-chromatography apparatus of claim 1, it is characterized in that said colloid keeps chromatographic column (1) and is the stainless steel chromatogram post of long 30-50mm, internal diameter 4-4.6mm, interface (21,22) at two ends is complementary with connecting pipe (11,16) about it, and stationary phase is the cyano bonded phase of 5-10 micron.
3. according to the said liquid-chromatography apparatus of claim 1, it is characterized in that said separation chromatography post (2) for about long 300mm, the stainless steel chromatogram post of internal diameter 4-10mm, the interface (23,24) and the connecting pipe (15,14) at two ends are complementary up and down for they, stationary phase can be selected from any in silica gel, aluminium oxide, the silica gel-aluminium oxide, and its granularity is the 5-40 micron.
4. according to the said liquid-chromatography apparatus of claim 1, connect according to interface 22 identical modes between the interface (21,22,23,24) that it is characterized in that chromatographic column (1,2) two ends and the connecting pipe, at first nut (22-3), sword ring (22-2) are enclosed within on the connecting pipe (16), connecting pipe (16) is inserted in the termination (22-1) of chromatographic column (1), load onto sword ring (22-2) then, use nut (22-3) to tighten at last.
5. according to the said liquid-chromatography apparatus of claim 1, it is characterized in that the stainless steel connecting pipe of said connecting pipe (10～20) for about 1/16 inch of external diameter.
6. according to the said liquid-chromatography apparatus of claim 1, it is characterized in that a hair dryer is equipped with as thermal source in the bottom of chromatographic column activation box (7), the thermocouple assay temperature is housed in the casing, by the heating of temperature controller control hair dryer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95206455 CN2227338Y (en) | 1995-03-28 | 1995-03-28 | Liquid chromatography device for separating dead oil component |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95206455 CN2227338Y (en) | 1995-03-28 | 1995-03-28 | Liquid chromatography device for separating dead oil component |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2227338Y true CN2227338Y (en) | 1996-05-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95206455 Expired - Fee Related CN2227338Y (en) | 1995-03-28 | 1995-03-28 | Liquid chromatography device for separating dead oil component |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2227338Y (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088605C (en) * | 1997-09-30 | 2002-08-07 | 中国科学院新疆化学研究所 | Quality control method for producing petroleum sodium sulfonate |
| CN101271094B (en) * | 2008-05-15 | 2011-06-01 | 宁波科宁达工业有限公司 | Zwitterion analysis system of ion chromatographic instrument |
| CN104165821A (en) * | 2014-08-01 | 2014-11-26 | 湖北富邦科技股份有限公司 | Method for determining colloid in wax oil |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN107262442A (en) * | 2017-08-01 | 2017-10-20 | 南京普氟生物检测技术有限公司 | It is a kind of to clean the method that sarpogrelate hydrochloride is remained in efficient liquid phase sampling valve |
| CN110196302A (en) * | 2018-02-27 | 2019-09-03 | 中国石油化工股份有限公司 | Automatic flushing device used in a kind of column chromatography adsorbing separation |
-
1995
- 1995-03-28 CN CN 95206455 patent/CN2227338Y/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088605C (en) * | 1997-09-30 | 2002-08-07 | 中国科学院新疆化学研究所 | Quality control method for producing petroleum sodium sulfonate |
| CN101271094B (en) * | 2008-05-15 | 2011-06-01 | 宁波科宁达工业有限公司 | Zwitterion analysis system of ion chromatographic instrument |
| CN104165821A (en) * | 2014-08-01 | 2014-11-26 | 湖北富邦科技股份有限公司 | Method for determining colloid in wax oil |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN104655768B (en) * | 2015-03-11 | 2016-08-17 | 天津博纳艾杰尔科技有限公司 | Oil component automatic separation equipment and the application in wax, colloid separation in crude oil thereof |
| CN107262442A (en) * | 2017-08-01 | 2017-10-20 | 南京普氟生物检测技术有限公司 | It is a kind of to clean the method that sarpogrelate hydrochloride is remained in efficient liquid phase sampling valve |
| CN110196302A (en) * | 2018-02-27 | 2019-09-03 | 中国石油化工股份有限公司 | Automatic flushing device used in a kind of column chromatography adsorbing separation |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| MM1K | Cease caused by non payment of annual fee |