CN1450349A - Quick petroleum hydrocarbon distribution analysis instrument - Google Patents
Quick petroleum hydrocarbon distribution analysis instrument Download PDFInfo
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- CN1450349A CN1450349A CN 02116828 CN02116828A CN1450349A CN 1450349 A CN1450349 A CN 1450349A CN 02116828 CN02116828 CN 02116828 CN 02116828 A CN02116828 A CN 02116828A CN 1450349 A CN1450349 A CN 1450349A
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- petroleum hydrocarbon
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Abstract
The invention is a quick distribution analyzer of petroleum hydrocarbon, including high-voltage electronic program step-up system with the pressure 0.2-1.0 MPa and the pressure programmed speed, 0.01-0.1 MPa/m, double-level filtering and diffluent sample-entering device, quartz capillary chromatogram column with the mixed stationary phase of SE-54 OV-1 in the inner wall, the proportion 1:(1-4) according to the weight shares, quick temperature programmed system with the temperature-increasing speed 20-60 deg.C/m, detector and the data processing system with the distribution of petroleum hydrocarbon and boiling-range distribution software system. The analyzer has quick speed and high resolution, and can be widely used in the fields such as oil, petrifaction, environmental protection and chemical industry.
Description
Technical field
The present invention puts it briefly and relates to a kind of analytical instrument, relates in particular to the quick petroleum hydrocarbon distribution analysis instrument of the various oil product special uses of a kind of former wet goods.
Background technology
Gas chromatograph is a kind of instrument in the analytical instrument, and it is mainly used in compartment analysis and inorganic and analysis organic gas potpourri of boiling point at the volatility organic mixture below 700 ℃.Name is called " the quick gas chromatograph of high pressure ", the patent No. is " ZL98249058.5 " number patent, the gas chromatograph that a kind of analysis speed is fast, resolution is high is disclosed, it has adopted high-pressure gas circuit system and high pressure super-resolution chromatographic column, make analysis speed improve 4～10 times, resolution has improved 4～6 times, thereby has saved analysis time widely, has improved resolution characteristic.But because it adopts is common high-pressure gas circuit system and temperature elevation system, so its analysis speed is still lower; It is a kind of general instrument that is widely used in every field such as oil, petrochemical industry, environmental protection, medicine, legal medical expert, chemical industry and agricultural simultaneously; if with the former wet goods oils of this instrumental analysis sample; the situation that chromatographic column is polluted, stopped up, damages takes place in regular meeting; and analysis speed is slow, and resolution is low.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, the quick petroleum hydrocarbon distribution analysis instrument of the various oil product special uses of former wet goods that a kind of analysis speed is fast, resolution is high is provided.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention comprises booster system, injector, chromatographic column, temperature elevation system, detecting device and data handling system.Wherein said temperature elevation system is the high-speed temperature programmed system.Described booster system is that programmed pressure is that 0.2～1.0Mpa, pressure program speed are 0.01～0.1MPa/ minute high-pressure electronic programmed pressure system, and it comprises gas cylinder, reduction valve, electron pressure operation valve and tensimeter.High-purity pressure gas N wherein is housed in the gas cylinder
2Or H
e, and be connected with reduction valve, reduction valve be linked in sequence electron pressure operation valve, tensimeter, injector, this injector connects electronic flow control valve and chromatographic column, chromatographic column connection detector.Described injector is the double-stage filtering split stream injector,, and it comprises main body, the upper cap nut that is connected with the main body upper and lower end respectively and following nut, places two silica gel dottle pins, central authorities disposing in turn from its upper end in the main body to have the dottle pin supporter and the internal lining pipe of through hole downwards.Fixedlying connected with main body in the upper end of described internal lining pipe, is provided with grade one filter and secondary filter in it from top to bottom.On the top wall of main body, have carrier gas inlet and at least two shuntings outlets that link to each other with the main body outer wall and communicate of being connected with the tensimeter outlet of described high-pressure electronic programmed pressure system with its inside, described each shunt to export and be communicated to the electronic flow control valve that flow is 30～200 ml/min.There is an infundibulate sample inlet in central authorities at upper cap nut, in the central authorities that descend nut one cylindrical hole are arranged.Described chromatographic column is passed described cylindrical hole and is connected with following nut.Described high-speed temperature programmed system heating rate is 20 ℃～60 ℃/minute, and temperature range is 50 ℃～350 ℃.Described chromatographic column for long 2～20 meters, 50～100 microns of internal diameters, inwall have SE-54 and OV-1 by weight ratio be 1: the Mixed Stationary of (1～4) quartzy capillary chromatograph mutually, the thickness of Mixed Stationary phase are 0.1～0.2 micron.Described detecting device is the small-size hydrogen flame ionization detector.Described data handling system has petroleum hydrocarbon and distributes and the boiling Range Distribution Analysis software systems.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, the programmed pressure of wherein said high-pressure electronic programmed pressure system is 0.4～0.8MPa, pressure program speed is 0.05MPa/ minute.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, wherein said high-speed temperature programmed system heating rate is 50 ℃/minute, temperature range is 80 ℃～320 ℃.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, the grade one filter of wherein said injector are silica wool, and secondary filter is the sintered quartz plate of 1 micron pore size, and the length ratio of grade one filter and secondary filter is 4: 1.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, wherein said chromatographic column inside coating thickness is 0.1 micron, the ratio of SE-54 and OV-1 is 1: 1.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, wherein quick petroleum hydrocarbon distribution analysis instrument is characterized in that described electronic flow control valve flow is 120 ml/min.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, wherein said hydrogen flame ionization detector have less than 0.1 milliliter of inner volume.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention, wherein said data handling system sample rate is 100 times/second.
The advantage and the good effect of quick petroleum hydrocarbon distribution analysis instrument of the present invention are: owing to adopted high-pressure electronic programmed pressure system and high-speed temperature programmed system, make oil and analysis of oil speed fast, again owing to be provided with grade one filter and secondary filter in the double-stage filtering split stream injector,, can filter colloid and bituminous matter in the former wet goods petroleum products, unlikely pollution also damages chromatographic column and detecting device; The chromatographic column inwall scribbles SE-54 and OV-1 Mixed Stationary mutually in addition, has improved resolution, guarantees that oil sample press the outflow of boiling point order.
Other details of quick petroleum hydrocarbon distribution analysis instrument of the present invention and characteristics can just can be cheer and bright by reading the embodiment hereinafter encyclopaedize in conjunction with the accompanying drawings.
Description of drawings
Fig. 1 be quick petroleum hydrocarbon distribution analysis instrument of the present invention process flow diagram;
Fig. 2 is the use principle figure of quick petroleum hydrocarbon distribution analysis instrument of the present invention;
Fig. 3 is the cut-open view that the double-stage filtering in the quick petroleum hydrocarbon distribution analysis instrument of the present invention amplifies injector.
Embodiment
Referring to Fig. 1.Fig. 1 be quick petroleum hydrocarbon distribution analysis instrument of the present invention process flow diagram.Sample is added the double-stage filtering split stream injector,, and the double-stage filtering split stream injector, is boosted in system by the high-pressure electronic programmed pressure, and most of after filtration sample is flowed out by the shunting outlet of electronic flow control valve; The quartzy capillary chromatograph that the high-speed temperature programmed system that enters another fraction heats up separates; After hydrogen flame ionization detector detected, data were input to data handling system and handle again.
Referring to Fig. 2.Quick petroleum hydrocarbon distribution analysis instrument of the present invention, it is circumscribed with source of the gas at Instrument shell is 15MPa high-pressure cylinder 1, and high-purity gas N is housed in the high-pressure cylinder 1
2Or H
eWhen making sample analysis with crude oil, open steel cylinder 1 controlled valve and high-pressure pressure-reducing valve 2 in the high-pressure electronic programmed pressure system, pressure is adjusted to 0.8MPa, regulate electron pressure operation valve 3 to 0.4MPa, rate of pressure rise is 0.05MPa/ minute; Regulate bypass flow electronic flow control valve 6 to 120 ml/min in the double-stage filtering split stream injector; Regulating high-speed temperature programmed device 9 is 80 ℃, and heating rate is 50 ℃/minute.Volatilization hydrocarbon component enters quartzy capillary chromatograph 7 by injector 5 in the crude oil, and hydrocarbon component flows out to hydrogen flame ionization detector 8 by the separation of boiling point order fast, and detection signal is handled through data handling system 10 and obtained hydrocarbon distributed data and boiling range data.Wherein the inner volume of hydrogen flame ionization detector is less than 0.1 milliliter.
Referring to Fig. 3.The double-stage filtering split stream injector, of quick petroleum hydrocarbon distribution analysis instrument of the present invention comprises main body 8, the upper cap nut 9 that is connected with main body 8 upper and lower ends respectively and following nut 10, places two silica gel dottle pins 11, central authorities disposing in turn from its upper end in the main body 8 to have the dottle pin supporter 12 and the internal lining pipe 13 of through hole downwards.Fixedlying connected with main body 8 in the upper end of internal lining pipe 13, is provided with grade one filter 14 and secondary filter 15 in it from top to bottom.Wherein grade one filter 14 can be a silica wool, secondary filter 15 can be that the aperture is 1 micron a sintered quartz plate, the length ratio of grade one filter and secondary filter can be 4: 1, and the effect of filtrator is to prevent contaminating impurity such as colloid in the former wet goods sample or bituminous matter or damages chromatographic column and detecting device.The effect of silica gel dottle pin is to guarantee injector impermeability under high pressure.Have on the top wall of main body 8 that the carrier gas inlet 16 that is connected with tensimeter 4 outlet of high-pressure electronic programmed pressure system links to each other with main body 8 outer walls with two and the shunting outlet that communicates with its inside, each shunting exports and is communicated to the electronic flow control valve 6 that flow is 30～200 ml/min.There is an infundibulate sample inlet in central authorities at upper cap nut 9, in the central authorities that descend nut 10 one cylindrical hole are arranged; Chromatographic column 7 is passed cylindrical hole and is connected with following nut 10.Chromatographic column 7 has SE-54 and OV-1 Mixed Stationary quartzy capillary chromatograph mutually for 10 meters of length, 75 microns of internal diameters, inwall, and inside coating thickness is 0.1 micron, and its coating thickness all is feasible in 0.1～0.2 micrometer range; The ratio of SE-54 and OV-1 is counted 1: 1 by weight, and its proportional range is 1: all be feasible between (1～4); Chromatographic column 7 length are at 2～20 meters, and internal diameter all is feasible at 50～100 microns.Wherein the component of SE-54 is 5% phenyl and 95% methyl polysiloxane, and the component of OV-1 is a polymethyl siloxane.
When carrying out compartment analysis with quick petroleum hydrocarbon distribution analysis instrument of the present invention, at first crude oil or petroleum product samples are sucked in the micro syringe, then this syringe is inserted through infundibulate sample inlet, pass the center through hole of double-deck silica gel dottle pin 11 and dottle pin supporter 12 and deliver to first order filtrator 14 and second level filtrator 15, inject the above-mentioned sample of 0.2 microlitre, this sample is being heated to 350 ℃, evaporation in first order filtrator 14, residue is left on first in the crude oil, in the secondary filter, after volatile hydrocarbon enters the quartzy capillary chromatograph 7 of super-resolution and separates by 1000: 1 split ratio, carry out data processing to detecting device 17 detections and by data handling system 18, remainder is discharged through electronic flow control valve 6.
Quick petroleum hydrocarbon distribution analysis instrument of the present invention can be widely used in neighborhoods such as oil, petrochemical industry, environmental protection, chemical industry, volatile hydrocarbon distribution, boiling range scope etc. in analyse crude oil, various oil product, the solvent wet goods extract can become that a kind of consumption is big, the medium-sized dedicated analysis instrument of wide application.
Claims (10)
1. quick petroleum hydrocarbon distribution analysis instrument, comprise booster system, injector, chromatographic column, temperature elevation system, detecting device and data handling system, it is characterized in that described temperature elevation system is the high-speed temperature programmed system, wherein said booster system is that programmed pressure is that 0.2～1.0Mpa, pressure program speed are 0.01～0.1MPa/ minute high-pressure electronic programmed pressure system, it comprises gas cylinder (1), reduction valve (2), electron pressure operation valve (3) and tensimeter (4), wherein in the gas cylinder (1) high-purity pressure gas N is housed
2Or H
e, and be connected with reduction valve (2), reduction valve (2) be linked in sequence electron pressure operation valve (3), tensimeter (4), injector (5), this injector (5) connects electronic flow control valve (6) and chromatographic column (7), chromatographic column (7) connection detector (17); Described injector (5) is the double-stage filtering split stream injector,, it comprises main body (8), respectively with main body (8) on, upper cap nut (9) and following nut (10) that the lower end connects, place the two silica gel dottle pins (11) that dispose in turn from its upper end in the main body (8) downwards, central authorities have the dottle pin supporter (12) and the internal lining pipe (13) of through hole, fixedly connected with main body (8) in the upper end of described internal lining pipe (13), be provided with grade one filter (14) and secondary filter (15) in it from top to bottom, having carrier gas inlet (16) and at least two shuntings that link to each other with main body (8) outer wall and communicate with its inside of being connected with tensimeter (4) outlet of described high-pressure electronic programmed pressure system on the top wall of main body (8) exports, described each shunting outlet is communicated to the electronic flow control valve that flow is 30～200 ml/min (6), there is an infundibulate sample inlet in central authorities at upper cap nut (9), in the central authorities that descend nut (10) one cylindrical hole are arranged; Described chromatographic column (7) is passed described cylindrical hole and is connected with following nut (10); Described high-speed temperature programmed system heating rate is 20 ℃～60 ℃/minute, and temperature range is 50 ℃～350 ℃; Described chromatographic column for long 2～20 meters, 50～100 microns of internal diameters, inwall have SE-54 and OV-1 by weight ratio be 1: the Mixed Stationary of (1～4) quartzy capillary chromatograph mutually, the thickness of Mixed Stationary phase are 0.1～0.2 micron; Described detecting device (17) is the small-size hydrogen flame ionization detector; Described data handling system has petroleum hydrocarbon and distributes and the boiling Range Distribution Analysis software systems.
2. quick petroleum hydrocarbon distribution analysis instrument according to claim 1 is characterized in that the programmed pressure of described high-pressure electronic programmed pressure system is 0.4～0.8MPa, and pressure program speed is 0.05MPa/ minute.
3. quick petroleum hydrocarbon distribution analysis instrument according to claim 1 and 2 is characterized in that described high-speed temperature programmed system heating rate is 50 ℃/minute, and temperature range is 80 ℃～320 ℃.
4. quick petroleum hydrocarbon distribution analysis instrument according to claim 1 and 2, the grade one filter (14) that it is characterized in that described injector is silica wool, secondary filter (15) is the sintered quartz plate of 1 micron pore size, and the length ratio of grade one filter (14) and secondary filter (15) is 4: 1.
5. quick petroleum hydrocarbon distribution analysis instrument according to claim 3, the grade one filter (14) that it is characterized in that described injector is silica wool, secondary filter (15) is the sintered quartz plate of 1 micron pore size, and the length ratio of grade one filter (14) and secondary filter (15) is 4: 1.
6. quick petroleum hydrocarbon distribution analysis instrument according to claim 3 is characterized in that described chromatographic column inside coating thickness is 0.1 micron, and the ratio of SE-54 and OV-1 is 1: 1.
7. according to the described quick petroleum hydrocarbon distribution analysis instrument of claim 1,2 or 5, it is characterized in that described chromatographic column inside coating thickness is 0.1 micron, the ratio of SE-54 and OV-1 is 1: 1.
8. quick petroleum hydrocarbon distribution analysis instrument according to claim 7 is characterized in that described electronic flow control valve flow is 120 ml/min.
9. according to claim 1,2,5,6 or 8 described quick petroleum hydrocarbon distribution analysis instruments is characterized in that described hydrogen flame ionization detector has less than 0.1 milliliter of inner volume.
10. quick petroleum hydrocarbon distribution analysis instrument according to claim 9 is characterized in that described data handling system sample rate is 100 times/second.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02116828 CN1213297C (en) | 2002-04-10 | 2002-04-10 | Quick petroleum hydrocarbon distribution analysis instrument |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02116828 CN1213297C (en) | 2002-04-10 | 2002-04-10 | Quick petroleum hydrocarbon distribution analysis instrument |
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|---|---|
| CN1450349A true CN1450349A (en) | 2003-10-22 |
| CN1213297C CN1213297C (en) | 2005-08-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 02116828 Expired - Fee Related CN1213297C (en) | 2002-04-10 | 2002-04-10 | Quick petroleum hydrocarbon distribution analysis instrument |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301406C (en) * | 2004-05-27 | 2007-02-21 | 上海烟草（集团）公司 | Automatic multi-dimensional gas-phase chromatographic system and use with non-valve pressure switching |
| CN1308678C (en) * | 2005-04-21 | 2007-04-04 | 张刘平 | Soil adsorbed hydrocarbon low-temperature desorption apparatus and method |
| CN102214491A (en) * | 2010-04-07 | 2011-10-12 | 通用电气-日立核能美国有限责任公司 | Column geometry to maximize elution efficiencies for molybdenum-99 |
| CN108389773A (en) * | 2018-03-22 | 2018-08-10 | 北京雪迪龙科技股份有限公司 | A kind of headspace sampling device and headspace sampling analysis system and method |
| CN112834633A (en) * | 2020-12-28 | 2021-05-25 | 北京杰宇广谱科技有限公司 | Fast hydrocarbon composition analyzer |
| CN112834634A (en) * | 2020-12-28 | 2021-05-25 | 北京杰宇广谱科技有限公司 | Fast gas chromatograph |
-
2002
- 2002-04-10 CN CN 02116828 patent/CN1213297C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301406C (en) * | 2004-05-27 | 2007-02-21 | 上海烟草（集团）公司 | Automatic multi-dimensional gas-phase chromatographic system and use with non-valve pressure switching |
| CN1308678C (en) * | 2005-04-21 | 2007-04-04 | 张刘平 | Soil adsorbed hydrocarbon low-temperature desorption apparatus and method |
| CN102214491A (en) * | 2010-04-07 | 2011-10-12 | 通用电气-日立核能美国有限责任公司 | Column geometry to maximize elution efficiencies for molybdenum-99 |
| US9240253B2 (en) | 2010-04-07 | 2016-01-19 | Ge-Hitachi Nuclear Energy Americas Llc | Column geometry to maximize elution efficiencies for molybdenum-99 |
| CN108389773A (en) * | 2018-03-22 | 2018-08-10 | 北京雪迪龙科技股份有限公司 | A kind of headspace sampling device and headspace sampling analysis system and method |
| CN112834633A (en) * | 2020-12-28 | 2021-05-25 | 北京杰宇广谱科技有限公司 | Fast hydrocarbon composition analyzer |
| CN112834634A (en) * | 2020-12-28 | 2021-05-25 | 北京杰宇广谱科技有限公司 | Fast gas chromatograph |
| CN112834634B (en) * | 2020-12-28 | 2022-10-04 | 北京杰宇广谱科技有限公司 | Fast gas chromatograph |
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| CN1213297C (en) | 2005-08-03 |
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