CN1245288A - Method and equipment for measuring the components and their contents of crude oil sample - Google Patents
Method and equipment for measuring the components and their contents of crude oil sample Download PDFInfo
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- CN1245288A CN1245288A CN 98117330 CN98117330A CN1245288A CN 1245288 A CN1245288 A CN 1245288A CN 98117330 CN98117330 CN 98117330 CN 98117330 A CN98117330 A CN 98117330A CN 1245288 A CN1245288 A CN 1245288A
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Abstract
A method for measuring the components and content in crude oil sample by determining the fluorescent spectrum distribution features that the components in crude oil sample can be determined by integrating the different wave bands of crude oil sample to be measured and the content of crude oil sample can be found out by integrating the particular wave band of fluorescent spectrum generated by the crude oil sample dissolved in solvent and comparing it with the integration of fluorescent spectrum of reference sample. Its equipment is composed of light source, optical filter, focusing system, monochrometor, detector, amplifier and computer.
Description
The invention belongs to optical technical field, relate to a kind of detection method and device of measuring crude oil sample content and composition with measurement fluorescence spectrum location mode.
The Chinese patent 89104984.3 of U.S. Tyke Sa Li development company, it is that emitting fluorescence with corresponding emitting fluorescence curve of known hydrocarbonaceous amount sample and solvate sample compares to determine tested crude oil test sample product hydrocarbonaceous amount, it only discloses a kind ofly detects determining the method for hydrocarbonaceous amount in the rock stratum underground rock stratum sample, and it can not be measured the composition in the tested crude oil sample.
The fluorospectrophotometer (RF-540) that Shimadzu Seisakusho Ltd. of Amada Co., Ltd. produces is as shown in Figure 1: it is by light source 1, concave mirror 2, monochromator 3, beam splitter 4, reference detector 5, condenser 6, sample 7, condenser 8, monochromator 9, concave mirror 10, detector 11 is formed, light source 1 sends radiant light and enter exciting light monochromator 3 behind concave mirror 2, produce monochromatic radiation after monochromator 3 beam split and produce two monochromic beams through beam splitter 4, a branch of reference detector 5 that enters, another route condenser 6 focuses on the sample 7, focused on the entrance slit of monochromator 9 behind the generation fluorescence by condenser 8, the monochromatic fluorescence that monochromator 9 produces focuses on detector 11 by concave mirror 10.The problem that its exists: its exciting light is by monochromator splitting, makes instrument cost height, and volume is big, and be not suitable for situ of drilling well and use, and its complex structure, to the environmental requirement height, running program is loaded down with trivial details; Condenser 6 and 8 at exciting light and fluorescence two places all adopts lens, limits because of lens material, makes that the transmitance below 300nm is lower, has limited instrument and has used wavelength band.
The objective of the invention is to overcome the not problem of energy measurement crude oil sample composition of prior art; Overcome that laser is sent out the instrument cost height that brought by monochromator splitting, volume is big, running program is loaded down with trivial details, be unsuitable for the problem that situ of drilling well uses; It is low in the following wave band transmitance of 300nm to overcome the lens type condenser system, has limited the problem of instrument use wavelength band.
Method of the present invention be with the monochromatic ultraviolet excitation light irradiation to the solvate crude oil sample, the present invention draws the light emission luminance value of known standard spectrum the calibration function of checkout equipment divided by measure the pairing light emission luminance value of known standard spectrum with checkout equipment; Deposit calibration function in computing machine, the crude oil sample fluorescence spectrum photosignal that records each time with calibration function and checkout equipment multiplies each other, and draws the corresponding fluorescence spectrum of crude oil sample and distributes; Distributing to distribute with the fluorescence spectrum of the identical wave band of crude oil sample with known crude oil sample fluorescence spectrum compares behind the integration respectively, obtains the hydrocarbonaceous amount of crude oil sample; At two different-waveband scope integrations, the integrated value to two different-waveband scopes compares then, obtains the Main Ingredients and Appearance of crude oil sample with the fluorescence spectrum intensity distributions of crude oil sample.
Device of the present invention is as shown in Figure 2: it comprises light source 1, optical filter 2, sample 3, condenser system 4, monochromator 5, main detector 6, amplifier 7, A/D converter 8, stepper motor driver 9, catoptron 10, optical filter 11, reference detector 12, amplifier 13, A/D converter 14, single-chip microcomputer 15, panel control 16, computer interface 17, base 18, multi-purpose computer 19, device of the present invention is being settled on the base 18: settle catoptron 10 and optical filter 2 respectively on two emergent raies at light source 1, optical filter 11 is settled on the opposite of catoptron 10, reference detector 12 is placed in back at optical filter 11, the output terminal of reference detector 12 connects with the input end of amplifier 13, the output terminal of amplifier 13 connects with the input end of A/D converter 14, settle reflecting condensation system 4 on the emitting light path of sample 3, the output beam of reflecting condensation system 4 feeds the entrance slit of monochromator 5.
Dynamic process of the present invention: a route light source 1 emission light shines on the optical filter 11 through catoptron 10 and produces the monochromatic light of specific wavelength, and shines reference detector 12, feeds A/D converter 14 through amplifier 13.Come the detection fluorescence spectrum signal value of naturalization main detector 6 acquisitions with the photosignal of reference detector 12.The light of another route light source 1 mating plate 2 after filtration produces monochromatic light, monochromatic light is radiated at and makes its generation fluorescence enter monochromator 5 through reflecting condensation system 4 on the sample 3, after the fluorescent radiation beam split of monochromator 5 with sample 3, the fluorescence spectrum of being surveyed sample 3 by main detector 6 distributes, and feeds A/D converter 8 by amplifier 7; Two signals at A/D converter 8 input ends are the photosignals that detect with the photosignal naturalization main detector 6 that reference detector 12 detects.Receive the photosignal of A/ D converters 8 and 14 by single-chip microcomputer 15, single-chip microcomputer 15 is finished data acquisition, the processing of fluorescence spectrum, the data transmission of fluorescence spectrum scanning.Step actuator 9 drives the scanning of the grating realization fluorescence spectrum of monochromator 5.The work order of panel control 16 input instruments is finished the instrument fluorescence spectrum and is detected.15 pairs of single-chip microcomputers detect data to carry out feeding computing machine 19 by computer interface 17 after the rough handling.The fluorescence spectrum distribution that main detector 6 records is sent into single-chip microcomputer 15 and multi-purpose computer 19 by A/D converter 8, spectral intensity distribution integration by 19 pairs of specific band scopes of computing machine, compare with benchmark crude sample integrated curve and crude oil sample integrated curve to be measured, can obtain the content of crude oil sample to be measured.The different-waveband that the fluorescence spectrum of crude oil sample to be measured is distributed carries out integration, and different-waveband is carried out integration relatively, can judge the composition of crude oil sample.
Good effect of the present invention: 1. adopt optical filter 2 to do the exciting light beam splitter, overcome the problem that the prior art monochromator brings, reduce the instrument volume, improve stability of instrument, reliability.2. gather reference light with catoptron 10 and enter the size that to dwindle used optical filter 11 with reference to detection device 12.3. the photosignal that detects of the reference signal naturalization main detector 6 that collects with reference detector 12 is eliminated the error of being brought because of light source and Circuits System instability.4. with computer interface the naturalization processing signals is transferred in the multi-purpose computer 19, naturalization specific band spectral distribution Integral Processing.And with solvate crude oil sample spectral distribution integrated value and the comparison of benchmark crude sample integrated value, can be in the hope of crude oil sample content to be measured.5. the present invention can carry out integration to the different-waveband of measured crude oil sample to be measured, and relatively determines the crude oil composition by the different-waveband integrated value.6. adopt the reflecting condensation system to overcome the little restriction of prior art lens light gathering system wavelength band, enlarged the wavelength band that instrument uses, improved service efficiency.
Description of drawings:
Fig. 1 is the prior art structural representation
Fig. 2 is a structure vertical view of the present invention
Fig. 3 is a structural principle block diagram of the present invention
One embodiment of the present of invention: light source 1 adopts mercury spectral lamp or other ultraviolet source, and optical filter 2 and 11 adopts wavelength to be: 254nm or 365nm, or other ultraviolet filter, and they have stronger line spectrum radiation at ultraviolet band, and bandwidth is: about 10nm.Reflecting condensation system 4 selects two catoptrons that the ultraviolet band reflectivity is higher for use.Monochromator 5 selects its wavelength band at 200-700nm, resolution 1nm.Main detector 6 and reference detector 12 are selected R928 model photomultiplier, at the 200-700nm wave band higher sensitivity is arranged, and change of sensitivity are mild.The minimum current that amplifier 7 and 13 can be selected to survey is 10nA, dynamic range 10
3A/ D converter 8 and 14 is selected 12 A/D converters.Stepper driver 9 comprises pulse producer and power amplification etc.Catoptron 10 usefulness glass are aluminized and are made.Single-chip microcomputer 15 is selected 8031 single-chip microcomputers for use.Panel control 16 is made up of numerical key and function key.Computer interface is selected the RS-232 serial line interface for use.Base 18 cast aluminiums are made.Computing machine 19 can be selected common PC computing machine for use.
The present invention adopts mercury lamp to make excitation source, and be used narrow band pass filter and produce mercury line and several excitation wavelengths, as 254nm, 365nm, 296nm etc., they have stronger line spectrum radiation at ultraviolet band, can produce good monochromatic excitation light behind optical filter.Excitation light irradiation produces fluorescence to the solvate sample, survey the fluorescence that is produced on vertical exciting light direction.Fluorescence is by the reflecting condensation systematic collection, and focus on the entrance slit of monochromator, detect the photosignal of sample by photomultiplier and photosignal that reference detector collects is divided by behind monochromator splitting, deduction is because of measuring error that flashing produced.The present invention scans crude oil sample to be measured and distributes in the fluorescence Spectra that burst of ultraviolel light source irradiation back produces, and judges Main Ingredients and Appearance and the content that crude oil to be measured is contained according to distribution character.
For detection by quantitative crude oil sample content to be measured, composition at the scene, need measure and be stored in computing machine to the representational known crude oil standard series comparative sample that detects the area, be used to demarcate the crude oil sample of unknown content composition.The contrast of every cover crude oil standard spectrum series divides 15 grades usually.It is as follows that known crude oil sample detects step:
1. according to oil property, different known crude oil standard series comparative sample is measured, and according to the difference of known crude oil sample, respectively the known sample fluorescence spectrum is carried out integration (can select the 250-700nm wave band for use usually), measure and being spaced apart of sampling that integration interval can be selected for use respectively according to known crude oil sample fluorescence spectrum distribution situation: 2nm, 5nm, 10nm, 20nm, the common mild sample of spectral distribution, sampling and integration interval can be selected greatly, and opposite sampling interval is littler.
2. standard series comparative sample fluorescence spectrum integrated value and known crude oil sample rank and content are mapped, simulate a crude oil rank and the crude content change curve with fluorescence spectrum intensity distributions integrated value, the fluorescence spectrum intensity distributions integrated value of being measured by crude oil sample to be measured is obtained the rank and the content of crude oil.
Crude oil sample to be measured detects step:
1. the solvate of known volume crude oil sample to be measured is put into the crude oil composition, in the content measurement device sample cell, the fluorescence spectrum of measuring it distributes, and it is carried out integration in specific spectral band scope, and integration interval is consistent with benchmark crude series comparative sample with wave band.This just can find out the crude oil composition and the content value of corresponding testing sample spectral intensity integrated value from known matched curve.
2. respectively the fluorescence spectrum distribution different-waveband of crude oil sample to be measured is carried out integration, as all band, ultraviolet light wave band, blue streak wave band, green light band, yellow band and red spectral band, and these integrated values are compared evaluation, can judge the crude oil composition according to proportionate relationship between the different-waveband.
Claims (2)
1. measuring method to crude oil sample composition and content, it be with the monochromatic ultraviolet excitation light irradiation to the solvate crude oil sample, it is characterized in that: the calibration function that the light emission luminance value of known standard spectrum is drawn checkout equipment divided by measure the pairing light emission luminance value of known standard spectrum with checkout equipment; Deposit calibration function in computing machine, the crude oil sample fluorescence spectrum photosignal that records each time with calibration function and checkout equipment multiplies each other, and draws the corresponding fluorescence spectrum of crude oil sample and distributes; Distributing to distribute with the fluorescence spectrum of the identical wave band of crude oil sample with known crude oil sample fluorescence spectrum compares behind the integration respectively, obtains the hydrocarbonaceous amount of crude oil sample; At two different-waveband scope integrations, the integrated value to two different-waveband scopes compares then, obtains the Main Ingredients and Appearance of crude oil sample with the fluorescence spectrum intensity distributions of crude oil sample.
2. the device that method according to claim 1 is made, it comprises light source 1, sample 3, monochromator 5, main detector 6, amplifier 7, A/D converter 8, stepper motor driver 9, single-chip microcomputer 15, panel control 16, computer interface 17, base 18, multi-purpose computer 19, it is characterized in that: settling on the base 18: settle catoptron 10 and optical filter 2 respectively on two emergent raies at light source 1, optical filter 11 is settled on the opposite of catoptron 10, reference detector 12 is placed in back at optical filter 11, the output terminal of reference detector 12 connects with the input end of amplifier 13, the output terminal of amplifier 13 connects with the input end of A/D converter 14, settle reflecting condensation system 4 on the emitting light path of sample 3, the output beam of reflecting condensation system 4 feeds the entrance slit of monochromator 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98117330 CN1103446C (en) | 1998-08-17 | 1998-08-17 | Method and equipment for measuring the components and their contents of crude oil sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98117330 CN1103446C (en) | 1998-08-17 | 1998-08-17 | Method and equipment for measuring the components and their contents of crude oil sample |
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| CN1245288A true CN1245288A (en) | 2000-02-23 |
| CN1103446C CN1103446C (en) | 2003-03-19 |
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| CN 98117330 Expired - Fee Related CN1103446C (en) | 1998-08-17 | 1998-08-17 | Method and equipment for measuring the components and their contents of crude oil sample |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451625C (en) * | 2006-06-23 | 2009-01-14 | 厦门大学 | Quantitative fluorescent logging method for expanding crude-oil linear analysis range |
| CN100460858C (en) * | 2005-12-13 | 2009-02-11 | 上海神开石油化工装备股份有限公司 | Method for on-line spectral determining oily gas in drilling liquid |
| CN100489502C (en) * | 2005-06-29 | 2009-05-20 | 赵菊英 | Method for making oil content in water measured by fluorescence method compared to other methods |
| CN101467025B (en) * | 2006-07-04 | 2011-03-02 | 东亚Dkk株式会社 | Oil type discrimination method and oil type discriminator |
| CN104508458A (en) * | 2012-05-25 | 2015-04-08 | 美卓自动化有限公司 | Sheet measurement |
| CN107250771A (en) * | 2015-01-05 | 2017-10-13 | 沙特阿拉伯石油公司 | Pass through fluorescent spectrometry analysis and characterization crude oil and its fraction |
| CN107589101A (en) * | 2017-09-28 | 2018-01-16 | 中国石油天然气集团公司 | Online oil-polluted water detection means based on ultraviolet fluorescence method |
| 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 |
-
1998
- 1998-08-17 CN CN 98117330 patent/CN1103446C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100489502C (en) * | 2005-06-29 | 2009-05-20 | 赵菊英 | Method for making oil content in water measured by fluorescence method compared to other methods |
| CN100460858C (en) * | 2005-12-13 | 2009-02-11 | 上海神开石油化工装备股份有限公司 | Method for on-line spectral determining oily gas in drilling liquid |
| CN100451625C (en) * | 2006-06-23 | 2009-01-14 | 厦门大学 | Quantitative fluorescent logging method for expanding crude-oil linear analysis range |
| CN101467025B (en) * | 2006-07-04 | 2011-03-02 | 东亚Dkk株式会社 | Oil type discrimination method and oil type discriminator |
| CN104508458A (en) * | 2012-05-25 | 2015-04-08 | 美卓自动化有限公司 | Sheet measurement |
| US9574994B2 (en) | 2012-05-25 | 2017-02-21 | Metso Automation Oy | Sheet measurement |
| CN107250771A (en) * | 2015-01-05 | 2017-10-13 | 沙特阿拉伯石油公司 | Pass through fluorescent spectrometry analysis and characterization crude oil and its fraction |
| CN107250771B (en) * | 2015-01-05 | 2020-09-01 | 沙特阿拉伯石油公司 | Characterization of crude oil and its fractions by fluorescence spectroscopy analysis |
| 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 |
| CN107589101A (en) * | 2017-09-28 | 2018-01-16 | 中国石油天然气集团公司 | Online oil-polluted water detection means based on ultraviolet fluorescence method |
| CN107589101B (en) * | 2017-09-28 | 2023-08-22 | 中国石油天然气集团有限公司 | Online oily sewage detection device based on ultraviolet fluorescence method |
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|---|---|
| CN1103446C (en) | 2003-03-19 |
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