CN2723988Y - Quick detector for petroleum product quality - Google Patents

Quick detector for petroleum product quality Download PDF

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Publication number
CN2723988Y
CN2723988Y CN 200420023400 CN200420023400U CN2723988Y CN 2723988 Y CN2723988 Y CN 2723988Y CN 200420023400 CN200420023400 CN 200420023400 CN 200420023400 U CN200420023400 U CN 200420023400U CN 2723988 Y CN2723988 Y CN 2723988Y
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China
Prior art keywords
light
converter
petroleum products
sample chamber
instrument
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Expired - Fee Related
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CN 200420023400
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Chinese (zh)
Inventor
戴连奎
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN 200420023400 priority Critical patent/CN2723988Y/en
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Abstract

The utility model relates to a quick detector for the petroleum product quality, compising a laser device, a sample chamber, a miniature fiber spectrometer, a/D converter and a micro-computer. The sample chamber of the utility model is a box body with a light inlet hole and a light outlet hole. Petroleum sample bottles are arranged in the box. A long passing light filter and a fiber input interface are provided between the petroleum sample bottle and the light outlet hole. The excitation light generated by the laser device is irradiated to the petroleum sample bottle of the sample chamber. After the diffuse reflection light generated from the petroleum sample bottle passes through the long passing light filter to leach the rayleigh light which is the same frequency as the excitation light, after the diffuse reflection light generated from the petroleum sample bottle passes through the fiber input interface to focus again, the diffuse reflection light generated from the petroleum sample bottle passes through the fiber to connect to the miniature fiber spectrometer. After the output signal of the miniature fiber spectrometer passes through the A/D converter to convert into the digital quantity, the output signal of the miniature fiber spectrometer is connected to the micro-computer. The output data of the A/D converter is conducted to process by the micro-computer. The Raman spectrum of the petroleum sample to be measured is acquired. The quality index of the petroleum sample is calculated through the functional relation between the Raman spectrogram and the petroleum product quality index. The detector has the advantages of low cost, small volume and convenient carryover.

Description

A kind of petroleum products quality rapid determination instrument
Technical field
The utility model relates to the determinator of petroleum products quality index.
Background technology
The composition and the character of petroleum products (comprising: various petroleum fractions and intermediate product in gasoline, kerosene, diesel oil, lubricated wet goods final products and the petroleum refining process) are check and the major parameter of controlling its quality.With gasoline product and component gasoline is example, and its main quality index parameter comprises: boiling range, octane value, Reynolds vapour pressure, arene content, olefin(e) centent, benzene content, sulfur content etc.
For various petroleum products quality index, mostly adopt at present " standard analytical process ", promptly oil sample is carried out quantitative test according to the method for ASTM prescribed by standard.This class standard analytical approach is often very time-consuming, the analytical equipment costliness, and the line service amount is big, the maintenance cost height.In addition, the operating personnel that testing equipment often needs the complete test site of facility and has higher technical merit, inefficiency is difficult to satisfy needs of production.
In order to overcome the limitation of standard analytical process, many Modern Analytical Instrument, as sequential use such as high resolution gas chromatography, high performance liquid chromatography, mass spectrum, nuclear magnetic resonance, ultraviolet and infrared spectrums in petroleum product analysis, though they have had raising in various degree to the mensuration precision and the speed of some parameter, still can not be satisfactory aspect instrument cost, analysis speed.In recent years, along with the development of Chemical Measurement, near-infrared spectral analysis technology is subjected to paying attention to widely both at home and abroad.This alanysis method is calculated the oil quality index based on the funtcional relationship between spectrogram and the oil quality index again by measuring the near infrared spectrum data of oil sample to be measured, has that analysis efficiency height, analysis speed are fast, sample need not advantages such as pre-service.Near-infrared spectrometers need adopt semiconductor diode array or fourier transform technique to detect spectrum, is mainly external product at present, costs an arm and a leg; Simultaneously, because near-infrared absorption spectrum is overlapping serious, except that a small amount of index such as gasoline octane value, diesel cetane-number, unsatisfactory at present to the mensuration precision of a lot of Key Quality Indicator.
For the petroleum products quality analysis, Raman spectrum can also obtain the characteristic information of each organism group rich in the oil sample except the advantage that has near infrared spectrum and have, as at wave number 1000cm -1About occur sharp-pointed phenyl ring characteristic peak, at wave number 1650cm -1About the significant thiazolinyl characteristic peak that occurs.These characteristic peaks have directly reflected the content of each organism atomic radical in the oil sample.For this reason, people such as Cooper [1-3]The gasoline spectroscopic data that is obtained according to the fourier transform raman spectroscopy instrument, adopt the partial least square algorithm for estimating to set up the spectral model of character such as octane number, vapour pressure, oxygenates level, arene content, and obtained desirable analysis precision.Yet these high-resolution Raman spectrum analysis instrument are bulky, and price is very expensive.
List of references
[1]Cooper,J.B.et?al.Determination?of?octane?number?and?Reid?vapor?pressure?of?commercialpetroleum?fuels?using?FT-Raman?spectroscopy?and?partial?least-squares?regression?analysis.Analytical?Chemistry,1995,67:4096-4100
[2]Cooper,J.B.et?a1.Determination?of?weight?percent?oxygen?in?commercial?gasoline:Acomparison?between?FT-Rarnan,FT-IR,and?dispersive?near-IR?spectroscopies.AppliedSpectroscopy,1996,50(7):917-721
[3]Cooper,J.B.et?al.Comparison?of?near-IR,Raman,and?mid-IR?spectroscopies?for?thedetermination?of?BTEX?in?petroleum?fuels.Applied?Spectroscopy,1997,51(11):1613-1620
Summary of the invention
The purpose of this utility model provides that a kind of cost is low, and volume is little, portable petroleum products quality rapid determination instrument.
Petroleum products quality rapid determination instrument of the present utility model mainly comprises laser instrument, the sample chamber, micro fiber spectrometer, A/D converter and microcomputer, said sample chamber is the casing with light well and light hole, casing is built-in with the oil sample bottle, from the oil sample bottle to being provided with long pass filter and optical fiber input interface between the light hole, the oil sample bottle of the excitation light irradiation that laser instrument sends to the sample chamber, from diffusing that the oil sample bottle sends, behind the Reyleith scanttering light of long pass filter elimination and exciting light same frequency, after focusing on, the optical fiber input interface is connected to micro fiber spectrometer again by optical fiber, the output signal of micro fiber spectrometer is connected to the input end of A/D converter, and the output terminal of A/D converter is connected to microcomputer.By microcomputer the output data of A/D converter is carried out pre-service such as digital filtering and format conversion to obtain the Raman spectrum of oil sample to be measured, calculate the quality index of oil sample again based on the funtcional relationship between Raman spectrogram and the oil quality index.
The exciting light that above-mentioned laser instrument sends can be from the light well direct irradiation of sample chamber to the oil sample bottle; In order to improve the sensitivity of analyzer, also can the optical fiber output interface be set at the light well place of sample chamber, between laser instrument and optical fiber output interface, be connected optical fiber, the excitation light irradiation that laser instrument is sent by optical fiber is to the oil sample bottle.
Petroleum products quality rapid determination instrument provided by the utility model, because laser instrument can adopt the bigger middle low-power semi-conductor solid laser of live width, micro fiber spectrometer can adopt CCD type detector array, makes instrument cost under the prerequisite that guarantees test performance descend greatly.In addition, the utility model can adopt commercially available fixed light path, the micro fiber spectrometer of grating beam splitting, and machine system does not have movable member, strong interference immunity, and good stability, volume are urinated in carrying.The utility model adopts microcomputer that sample data is carried out pre-service, and sets up the Raman spectrum analysis computation model in real time, makes test speed improve greatly, can obtain the analysis result of the one or more quality index of testing sample in 1~2 minute.
Petroleum products quality rapid determination instrument provided by the utility model is applicable to petroleum products composition and quality index analysis, is specially adapted to light-end products, as gasoline, kerosene, liquefied gas etc., also can be used for light transmission other liquid-phase product preferably.Analyzable parameter comprises: the content (as the arene content in the oil product, olefin(e) centent, oxygenates level etc.) of the content of a certain material in the testing sample (as water cut, benzene content, drinks ethanol content etc.), certain class material and other overall target (as octane number, gasoline Reynolds vapour pressure, oil density etc.).
Description of drawings
Fig. 1 is a formation synoptic diagram of the present utility model;
Fig. 2 is a kind of concrete structure synoptic diagram of the utility model sample chamber;
Fig. 3 is the another kind of concrete structure synoptic diagram of the utility model sample chamber.
Embodiment
With reference to Fig. 1, the petroleum products quality rapid determination instrument that the utility model provides comprises laser instrument 1, sample chamber 3, micro fiber spectrometer 4, A/D converter 5 and microcomputer 6.Said sample chamber 3 is for to have the casing (see figure 2) of light well A and light hole B, and casing is built-in with oil sample bottle 9, from oil sample bottle 9 to being provided with long pass filter 11 and optical fiber input interface 12 between the light hole B.Internal memory the drain the oil oil sample bottle 9 of sample in sample chamber can be made with common optical glass or quartz material, and the also available metal material that has optical transmission window is made.Be to improve the signal to noise ratio (S/N ratio) of Raman spectrum, can be at sample chamber light well A wall or the inwall in the whole sample chamber are provided with light absorbent 10.Long pass filter 11 selects for use average transmission rate to the Raman light signal greater than 80% usually, and (OD5 is meant: after long pass filter filtered, its light intensity was reduced to 10 of former light intensity greater than OD5 to the dough softening of Reyleith scanttering light -5) optical filter, to improve the precision of analyzer.The excitation light irradiation that laser instrument 1 sends is to the oil sample bottle 9 of sample chamber, from diffusing that the oil sample bottle sends, behind the Reyleith scanttering light of long pass filter 11 eliminations and exciting light same frequency, after focusing on, optical fiber input interface 12 is connected to micro fiber spectrometer 4 by optical fiber 2 again from light hole B, the output signal of fiber spectrometer 4 is connected to the input end of A/D converter 5, and the output terminal of A/D converter 5 is connected to microcomputer 6.
Fig. 3 is the another kind of concrete structure synoptic diagram of sample chamber.Light well A place in the sample chamber is provided with optical fiber output interface 7, is connected optical fiber 2 between laser instrument 1 and optical fiber output interface 7, adopts excitation light irradiation that optical fiber 2 sends laser instrument 1 to the oil sample bottle.For other stray light beyond the filtering monochromatic excitation light, between laser instrument 1 and oil sample bottle 9, add narrow band pass filter 8 usually.In the instantiation shown in Figure 3, narrow band pass filter 8 places between optical fiber output interface 7 and the oil sample bottle 9.
In the utility model, said laser instrument 1 can be selected the middle low-power semi-conductor solid laser of wavelength in visible light or near-infrared region for use, as low-power semiconductor pump laser among the 532nm of domestic manufacturers' production, the 785nm semi-conductor solid laser that U.S. LaserPath technology company is produced.Because the Raman spectrum that above-mentioned laser instrument produced is in the shortwave near-infrared region, corresponding micro fiber spectrometer 4 can adopt CCD type detector array cheaply.Also can be commercially available for the A/D converter 5 that is used with the ccd array micro fiber spectrometer, as the ADC series of producing with U.S. OceanOptics company.A/D converter 5 can adopt USB interface, RS232 serial port or parallel port to be connected with microcomputer 6; Perhaps also A/D converter 5 can be placed in the slot of microcomputer 6, A/D converter 5 is connected with micro fiber spectrometer 4 with cable.A/D converter 5 also can be integrated in one with fiber spectrometer 4, as selects the A/D converter 5 of U.S. OceanOptics company production and USB2000, the HR2000 series of products that fiber spectrometer 4 is integrated in one for use.
In the utility model, said optical fiber output interface 7 can be made of the quartz lens and the fiber connector of adjustable focus respectively with optical fiber input interface 12, wherein fiber connector can adopt SMA 905, and standards such as ST or FC are concrete relevant with selected micro fiber spectrometer.Optical fiber output interface 7 also can be commercially available with optical fiber input interface 12, as 74 series of U.S. OceanOptics company production.
In the utility model, the optical fiber that connects usefulness can be selected common silica fibre for use.For guaranteeing logical light quantity, should select diameter to be not less than the optical fiber of 100 μ m.Micro fiber spectrometer 4 can be commercially available, as the S2000 micro fiber spectrometer of U.S. OceanOptics company production.
The microcomputer 6 that the utility model is used can be common desk-top or portable PC, or embedded computer, or other support the computing equipment (as programmable logic controller (PLC) etc.) of USB, RS232 interface.Microcomputer 6 is responsible for spectroscopic data is carried out pre-service and analytical calculation.Used analytical calculation software is based on the known standard oil sample database of quality index, adopt linearity and nonlinear mathematical model, and binding pattern sorting technique, set up the Quantitative Analysis Model of product quality indicator in real time, and directly calculate the spectral analysis value of its quality index by the Raman spectrum of oil sample to be measured.
The utility model also can be taked laser instrument 1, sample chamber 3, micro fiber spectrometer 4 and A/D converter 5 are placed same casing, and the top that is positioned at the sample chamber at casing is provided with a removable top cover, carries with more convenient.

Claims (11)

1. petroleum products quality rapid determination instrument, it is characterized in that mainly comprising laser instrument (1), sample chamber (3), micro fiber spectrometer (4), A/D converter (5) and microcomputer (6), said sample chamber (3) is for having the casing of light well (A) and light hole (B), casing is built-in with oil sample bottle (9), from oil sample bottle (9) to being provided with long pass filter (11) and optical fiber input interface (12) between the light hole B, the oil sample bottle (9) of the excitation light irradiation that laser instrument (1) sends to the sample chamber, from diffusing that the oil sample bottle sends, behind the Reyleith scanttering light of (11) elimination of long pass filter and exciting light same frequency, after focusing on, optical fiber input interface (12) is connected to micro fiber spectrometer (4) again by optical fiber (2), the output signal of micro fiber spectrometer (4) is connected to the input end of A/D converter (5), and the output terminal of A/D converter (5) is connected to microcomputer (6).
2. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that laser instrument (1) is a semi-conductor solid laser.
3. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that exciting light that laser instrument (1) sends from light well (A) direct irradiation of sample chamber to oil sample bottle (9); Perhaps the light well of (3) (A) locates to be provided with optical fiber output interface (7) in the sample chamber, is connected to be used for excitation light irradiation that laser instrument (1) the is sent optical fiber (2) to oil sample bottle (9) between laser instrument (1) and optical fiber output interface (7).
4. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that said optical fiber input interface (12) is made of the lens and the fiber connector of adjustable focus.
5. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that between laser instrument (1) and oil sample bottle (9), narrow band pass filter (8) being set.
6. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that wall or the inwall in the whole sample chamber being provided with light absorbent (10) at sample chamber light well (A).
7. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that micro fiber spectrometer (4) adopts CCD type detector array.
8. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that said A/D converter (5) and micro fiber spectrometer (4) are integrated in one; Or A/D converter (5) placed in the slot of microcomputer (6).
9. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that A/D converter (5) and microcomputer (6) adopt USB interface, RS232 serial port or parallel port to be connected.
10. by the described petroleum products quality rapid determination instrument of claim 1, it is characterized in that microcomputer (6) be common desk-top or portable PC, or the computing equipment of embedded computer or other supports USB, RS 232 interfaces; Said laser instrument (1), sample chamber (3), micro fiber spectrometer (4) and A/D converter (5) place same casing, and at the top that casing is positioned at the sample chamber one removable top cover are set.
11., it is characterized in that said optical fiber output interface (7) is made of the lens and the fiber connector of adjustable focus by the described petroleum products quality rapid determination instrument of claim 3.
CN 200420023400 2004-06-01 2004-06-01 Quick detector for petroleum product quality Expired - Fee Related CN2723988Y (en)

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Application Number Priority Date Filing Date Title
CN 200420023400 CN2723988Y (en) 2004-06-01 2004-06-01 Quick detector for petroleum product quality

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107787450A (en) * 2015-06-10 2018-03-09 沙特阿拉伯石油公司 Use induced with laser Ultraluminescence spectral characterization crude oil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107787450A (en) * 2015-06-10 2018-03-09 沙特阿拉伯石油公司 Use induced with laser Ultraluminescence spectral characterization crude oil

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C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20050907

Termination date: 20120601