CN100451625C - Quantitative fluorescent logging method for expanding crude-oil linear analysis range - Google Patents
Quantitative fluorescent logging method for expanding crude-oil linear analysis range Download PDFInfo
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Abstract
A quantitative fluorescence logging method to amplify the linear analysis range of the crude oil is provided in the invention. It prepares the 500-10000mg/L crude oil mother liquid using the normal hexane as the dissolvent; it dilutes the crude oil mother liquid to four parts of 5-300mg/L dilution crude oils. The dilution crude oil is put into the normal liquid bath or the thin liquid bath, then it is scanned by the fluorescence spectrometer with the constant energy isochronous scanning function in the vertical irradiation mode or the front surface irradiation mode to get the crude oil linear range. The linear range can reach to 300mg/L of the different crude oil.
Description
Technical field
The present invention relates to a kind of rationing fluorescent logging method, especially relate to a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope that adopts.
Background technology
The very complicated potpourri that oil is made up of chemical compound lot, its physical property and chemical property are also quite complicated and changeable.Crude oil is changeful to the tarry of black thickness from colourless liquid, and some at room temperature or even the solid shape.Because the existence of palycyclic aromatic, most of oil can both fluoresce, therefore, fluorescent technique can be used as quick, the nondestructive important means of analyzing oil, in numerous petroleum prospecting geologic logging methods, occupy a tiny space (1, Patra D, Mishra A K, Talanta, 2001,53:783; 2, Patra D, Mishra A K, Anal.Bioanal.Chem.2002,373:304.).
Aromatic hydrocarbon in the crude oil (promptly giving birth to glimmering group) is under excitation light irradiation, absorption of electromagnetic radiation can the back by ground state transition to unsettled excited state, when getting back to stable ground state by excited state again, unnecessary energy just discharges with the form of emitting fluorescence, can measure the content of oil according to the brightness of fluorescence, can measure the constituent of oil according to luminous color, the ultimate principle of Here it is fluorologging.
According to the evolution of detection hardware, the development course of fluorologging technology specifically can be divided into qualitative observation and two stages of quantitative test.Use conventional sense instrument (fluorescent light) range estimation deciding grade and level to analyze in the qualitative observation stage, easily miss the lightweight oil layer, the observed result subjectivity is strong, lacks science and practicality.Use the quantitative fluorescence detector in the quantitative test stage.At present, the quantitative fluorescence detector that use in domestic oil field generally adopts the ultraviolet excitation oil sample of 254nm, the fluorescent emission wavelength coverage that palycyclic aromatic produces in the oil under this excitation wavelength be 260～600nm (1, peace is civil and military, Su Jinlong, etc., the well logging technology, 2000,11 (4): 35; 2, Wang Zhizhan, the well logging technology, 2002,13 (1): 35), main peak appears at 300～400nm.This high-octane short wavelength's exciting light makes the fluorescence of palycyclic aromatic in the crude oil produce quencher easily, and the maximum excitation wavelength of this single not all palycyclic aromatic of excitation wavelength makes crude assay sensitivity greatly descend.
In the rationing fluorescent logging process; usually also run into problems such as inner filtering effect, energy transfer and spectral peak shift; make the range of linearity of quantitative test oil shorten greatly; can only be confined to just to have good linear relationship under the very low concentration; limited the quantitative test of oil, this problem is particularly serious for mink cell focus.Generally speaking, the range of linearity of crude oil between 0～40mg/L (Li Bin, Peng Chao, etc., record and technology, 2000,11 (4): 25),, measure again after must diluting for the sample that surpasses this scope.There is following several respects problem in this method: 1. wasted a large amount of reagent after many dilutions, increased expense; 2. because the use of a large amount of organic solvents, particularly unfavorable to the on-the-spot test personnel's that are in crawl space health; 3. in using drill bit rapid drilling process, because must carry out sample and repeatedly dilute, and repeatedly scan, whole mensuration process is loaded down with trivial details time-consuming, make on-the-spot sample determination speed may not satisfy the requirement of on-the-spot rapid drilling, can not reflect field condition rapidly and accurately.The limitation of the crude oil range of linearity has become the widely used bottleneck of fluorologging technology.
Summary of the invention
The objective of the invention is to above-mentioned many shortcomings, a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope is provided at existing fluorescent logging method existence.
Concrete steps of the present invention are:
1) preparation crude oil mother liquor:
For the solvent compound concentration is 500～10000mg/L, be preferably the crude oil mother liquor of 1000mg/L with the normal hexane;
2) preparation diluent crude oil solution:
Is at least 4 parts of diluent crude oil solution of concentration 5～300mg/L with the crude oil mother liquor for preparing with the normal hexane dilution;
3) quantitative fluorescence is measured and is obtained the crude oil range of linearity:
With conventional liquid pool or slim liquid pool, with vertical irradiation mode or front surface radiation modality, scanning constant-energy synchronous fluorescence spectrum obtains the crude oil range of linearity on the fluorospectrophotometer that has permanent energy synchronous scanning function with the diluent crude oil solution for preparing.
Described conventional liquid pool generally adopts the commercial conventional fluorescence liquid pool of 10mm * 10mm.
Described slim liquid pool generally is meant the slim fluorescence liquid pool of (1～5) mm * (10～30) mm.
Described front surface radiation modality is meant and allows exciting light become 20 °～40 ° or 55 °～70 ° with the liquid pool sensitive surface that preferably 30 ° of angles shine liquid pools.
The principle and the method for foundation of the present invention are as follows.
The constant-energy synchronous fluorescence method is that a branch of synchronous fluorimetry is (referring to document: 1, Inman E L, WinefordnerJr.J D, Anal.Chem., 1982,54:2018; 2, He L F, Lin D L, Li Y Q, Anal.Sci., 2005,21:641; 3, Li Y Q, Huang X Z, Xu J G, Chen G Z, Anal.Chim.Acta, 1992,256:285.), this method serves as according to carrying out synchronous scanning, making energy difference [(1/ λ that is maintained fixed between excitation wavelength and the emission wavelength in the scanning process with the characteristic energy of the quantum vibration transition of fluorophor
Ex-1/ λ
Cm)=Δ v=constant].The vibrational band of palycyclic aromatic is about 1400cm at interval
-1Though the accurate position of vibrational band may be subjected to displacement with the change of compound in the normal alkane solvent, its relative spacing remains unchanged substantially, so the constant-energy synchronous fluorescence method is particularly suitable for the discriminating and the mensuration of palycyclic aromatic.The constant-energy synchronous fluorescence method can show the useful information in the three-dimensional fluorescence spectrum information with two-dimensional signal, shorten the test duration greatly, and can in the spectrum that single pass obtains, select the less spectrum peak that influenced by fluorescent quenching to carry out quantitatively selectively.Therefore, the basic spectral scan pattern of the present invention adopts the constant-energy synchronous fluorescence method.
When the concentration of fluorescent material hour, fluorescence intensity is directly proportional with the concentration of fluorescent material, its relational expression is
F＝2.3KφI
0εbc (1)
In the formula (1), K---instrument parameter; F---relative intensity of fluorescence; φ---fluorescence efficiency; I
0---excitating light strength; ε---molar absorptivity, unit are L/mol/cm; B---light path, i.e. liquid layer thickness, unit is cm; The concentration of c---fluorescent material, unit is g/mL.At this moment satisfy ε bc＜0.05, ε bc is a dimensionless.
But when the concentration of fluorescent material is big (ε bc＞0.05), the linear relationship of fluorescence intensity and its concentration will depart from, and the shape and the position of fluorescence peak also change in the time of seriously.Its reason may be intermolecular the running foul of each other that excited and degradedness (self-quenching), or fluorescence is absorbed (self-absorption) by unexcited molecule again, most exciting light that also may be the highdensity molecule absorption of liquid pool previous section makes the molecule of back can not get exciting (inner filtering effect).
Satisfy the condition (ε bc＜0.05) of linear relationship from fluorescent material, can make the concentration c of fluorescent material satisfy ε bc＜0.05 in the larger context, thereby enlarge the range of linearity of fluorescence analysis by reducing b (promptly shortening light path).Adopt slim liquid pool (referring to Fig. 1), reduce liquid pool thickness, can shorten the light path that exciting light passes through; The front surface radiation modality is placed slim liquid pool 1 with have a certain degree with exciting light 2 (rather than traditional 90 °), make 2 irradiations of exciting light near behind one deck solution of liquid pool 1 very thin surface, most of reflected light 3 leaves liquid pool in the mode that is close to total reflection, and do not continue to excite the solution of back, detecting device 5 can reach the purpose that shortens light path equally receiving fluorescence 4 with the direction of 2 one-tenth 90 ° of exciting lights.Adopt slim liquid pool in conjunction with the front surface mode, can shorten the light path that exciting light passes through significantly, solve the inner filtering effect of heavy oil effectively, enlarge the range of linearity, improve linear relationship, help on-the-spot crude oil fast measuring.
The present invention is a solvent with the normal hexane on the fluorospectrophotometer that has permanent energy synchronous scanning function, and utilization constant-energy synchronous fluorescence method for lightweight oil and middle matter oil, adopts conventional liquid pool and vertical irradiation mode; For mink cell focus,, avoid crude oil high concentration quencher phenomenon by improving liquid pool and radiation modality.The present invention makes the range of linearity of different oil all can reach 300mg/L.
The fluorospectrophotometer that has a permanent energy synchronous scanning function can adopt the PERKIN ELMER LS-50B fluorospectrophotometer as the U.S., the multi-functional fluorospectrophotometer of MYF of VARIAN ECLIPSE type fluorospectrophotometer and China etc.
Description of drawings
The slim liquid pool front surface of the oil sample radiation modality synoptic diagram that Fig. 1 adopts for the present invention.
Fig. 2 is the constant-energy synchronous fluorescence spectrogram of 5 kinds of crude oil.In Fig. 2, curve a: white oil, b: middle matter crude oil, c: wooden crude oil, d:381 well crude oil, e: xinjiang crude oil.Horizontal ordinate is excitation wavelength (nm), and ordinate is a relative intensity of fluorescence.
Fig. 3 is for adopting the linear relationship curve of the conventional liquid pool of 10mm * 10mm white oil in 5～300mg/L concentration range.In Fig. 3 neutral line fit equation is Y=0.36X+1.76, and related coefficient is R=0.9976.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
Fig. 4 when adopting the conventional liquid pool of 10mm * 10mm in the linear relationship curve of matter crude oil.In Fig. 4 neutral line fit equation is Y=1.50X+1.17, and related coefficient is R=0.9991.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
The linear relationship curve of Fig. 5 wooden crude oil when adopting the conventional liquid pool of 10mm * 10mm.In Fig. 5 neutral line fit equation is Y=8.96X+36.59, and related coefficient is R=0.9975.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
The linear relationship curve of Fig. 6 381 well crude oil when adopting the conventional liquid pool of 10mm * 10mm is Y=3.56X+11.74 in Fig. 6 neutral line fit equation, and related coefficient is R=0.9981.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
The linear relationship curve of Fig. 7 xinjiang crude oil when adopting the conventional liquid pool of 10mm * 10mm is Y=6.50X+28.78 in Fig. 7 neutral line fit equation, and related coefficient is R=0.9986.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
Fig. 8 is the linear relationship curve of wooden crude oil when adopting the slim liquid pool front surface of 5mm * 20mm mode, is Y=11.07X+34.30 in Fig. 8 neutral line fit equation, and related coefficient is R=0.9970.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
Fig. 9 is the linear relationship curve of wooden crude oil when adopting the slim liquid pool front surface of 1mm * 20mm mode, is Y=2.84X+17.15 in Fig. 9 neutral line fit equation, and related coefficient is R=0.9981.Horizontal ordinate is concentration (mg/L), and ordinate is a relative intensity of fluorescence.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Is the white oil mother liquor of 1000mg/L with the normal hexane for the solvent compound concentration.Is the dilution white oil solution of concentration 5～300mg/L with the white oil mother liquor for preparing with the normal hexane dilution.
With conventional fluorescence liquid pool, in the vertical irradiation mode, scanning constant-energy synchronous fluorescence spectrum obtains the crude oil range of linearity on the fluorospectrophotometer that has permanent energy synchronous scanning function with the above-mentioned dilution white oil solution for preparing, and step is as follows:
1. it is 1400cm that the permanent energy synchronous scanning of fluorospectrophotometer wave-number difference is set
-1
2. the above-mentioned dilution white oil solution for preparing is poured into respectively in the conventional liquid pool of 10mm * 10mm, allowed exciting light shine liquid pool, according to the above-mentioned parameter scanning constant-energy synchronous fluorescence spectrum (referring to Fig. 2 a and Fig. 3) that sets with vertical mode.
3. the collection of illustrative plates after will scanning is preserved, and reads peak value, with data processing software match working curve (referring to Fig. 3).The range of linearity, linear fit equation and related coefficient are as shown in table 1.
Table 15 kind of crude oil linear fit parameter
Similar to Example 1, its difference is matter crude oil in the crude oil employing, and its result is referring to table 1 and Fig. 2 b and Fig. 4.
Similar to Example 1, its difference is that crude oil adopts wooden crude oil, and its result is referring to table 1 and Fig. 2 c and Fig. 5.
Similar to Example 1, its difference is that crude oil adopts 381 well crude oil, and its result is referring to table 1 and Fig. 2 d and Fig. 6.
Similar to Example 1, its difference is that crude oil adopts xinjiang crude oil, and its result is referring to table 1 and Fig. 2 e and Fig. 7.
As can be seen from the above embodiments, oil component is heavy more, and intensity is strong more, and inner filtering effect is also serious more, thereby the range of linearity is narrow more, and linearity is also poor more.In the concentration range of being investigated, adopt permanent energy synchronous scanning mode than the white oil of light constituent and middle matter crude oil, obtain good linear relationship, do not find tangible quencher phenomenon; Tangible quencher phenomenon has then taken place in the crude oil of other 3 kinds of heavy components, wherein especially with wooden crude oil for very.
Adopt slim liquid pool in conjunction with the front surface radiation modality, can shorten light path, solve the inner filtering effect of heavy oil, enlarge the range of linearity, improve linear relationship.
Following examples 6 and 7 adopt slim liquid pool to be used to investigate the most serious wooden crude oil of quencher in conjunction with the front surface radiation modality.
Embodiment 6
Similar to Example 3, its difference is to adopt the slim liquid pool of 5mm * 20mm (referring to Fig. 1), allows the former surface based fashion (exciting light becomes 30 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool, and its result is referring to table 1 and Fig. 2 c and Fig. 8.
Embodiment 7
Similar to Example 3, its difference is to adopt the slim liquid pool of 1mm * 20mm, allows the former surface based fashion (exciting light becomes 30 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool, and its result is referring to table 1 and Fig. 2 c and Fig. 9.
Shown in figure, the slim liquid pool of 5mm * 20mm has solved the quencher that causes because of inner filtering effect to a certain extent, and the range of linearity reaches 140mg/L than wide with conventional liquid pool; And the slim liquid pool of 1mm * 20mm has solved the quencher that inner filtering effect causes well, match in the 300mg/L scope, and related coefficient reaches 0.9981.
To sum up analyze, in fluorologging, adopt slim liquid pool front surface mode can solve the concentration effect problem effectively, thereby improve the working curve range of linearity.After using this method, even the most serious wooden crude oil of quencher also can have the better linearity relation in 5～300mg/L concentration range.
Embodiment 8
Similar to Example 1, it is the white oil mother liquor of 500mg/L that its difference is with the normal hexane to the solvent compound concentration.With the white oil mother liquor for preparing is 4 parts of dilution white oil solution of concentration 5～300mg/L with the normal hexane dilution.
With the above-mentioned dilution white oil solution for preparing with conventional fluorescence liquid pool, in the vertical irradiation mode, scanning constant-energy synchronous fluorescence spectrum on the fluorospectrophotometer that has permanent energy synchronous scanning function, obtain the crude oil range of linearity, in step 1, setting the permanent energy synchronous scanning of fluorospectrophotometer wave-number difference is 1100cm
-1
Embodiment 9
Similar to Example 1, it is the white oil mother liquor of 10000mg/L that its difference is with the normal hexane to the solvent compound concentration.With the white oil mother liquor for preparing is 4 parts of dilution white oil solution of concentration 5～300mg/L with the normal hexane dilution.
With the above-mentioned dilution white oil solution for preparing with conventional fluorescence liquid pool, in the vertical irradiation mode, scanning constant-energy synchronous fluorescence spectrum on the fluorospectrophotometer that has permanent energy synchronous scanning function, obtain the crude oil range of linearity, in step 1, it is 1600cm that the permanent energy synchronous scanning of fluorospectrophotometer wave-number difference is set
-1
Embodiment 10
Similar to Example 1, it is the white oil mother liquor of 2000mg/L that its difference is with the normal hexane to the solvent compound concentration.With the white oil mother liquor for preparing is 4 parts of dilution white oil solution of concentration 5～300mg/L with the normal hexane dilution.
With the above-mentioned dilution white oil solution that the prepares slim fluorescence liquid pool of 5mm * 10mm, surface irradiation mode in the past (exciting light becomes 30 ° of angles with the liquid pool sensitive surface), scanning constant-energy synchronous fluorescence spectrum on the fluorospectrophotometer that has permanent energy synchronous scanning function, obtain the crude oil range of linearity, in step 1, it is 1300cm that the permanent energy synchronous scanning of fluorospectrophotometer wave-number difference is set
-1
Embodiment 11
Similar to Example 3, its difference is to adopt the slim liquid pool of 5mm * 20mm, allows the former surface irradiation mode (exciting light becomes 20 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool.
Embodiment 12
Similar to Example 3, its difference is to adopt the slim liquid pool of 1mm * 20mm, allows the former surface irradiation mode (exciting light becomes 40 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool.
Embodiment 13
Similar to Example 3, its difference is to adopt the slim liquid pool of 1mm * 20mm, allows the former surface irradiation mode (exciting light becomes 55 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool.
Embodiment 14
Similar to Example 3, its difference is to adopt the slim liquid pool of 5mm * 20mm, allows the former surface irradiation mode (exciting light becomes 70 ° of angles with the liquid pool sensitive surface) of exciting light shine liquid pool.
Claims (9)
1. rationing fluorescent logging method that enlarges crude oil linear analysis scope is characterized in that its concrete steps are:
1) preparation crude oil mother liquor:
Is the crude oil mother liquor of 500～10000mg/L with the normal hexane for the solvent compound concentration;
2) preparation diluent crude oil solution:
Is at least 4 parts of diluent crude oil solution of concentration 5～300mg/L with the crude oil mother liquor for preparing with the normal hexane dilution;
3) quantitative fluorescence is measured and is obtained the crude oil range of linearity:
With conventional liquid pool or slim liquid pool, with vertical irradiation mode or front surface radiation modality, scanning constant-energy synchronous fluorescence spectrum obtains the crude oil range of linearity on the fluorospectrophotometer that has permanent energy synchronous scanning function with the diluent crude oil solution for preparing.
2. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 1 is characterized in that in step 1) described compound concentration is 1000mg/L.
3. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 1 is characterized in that in step 3), and described conventional liquid pool is 10mm * 10mm fluorescence liquid pool.
4. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 1 is characterized in that in step 3), and described slim liquid pool is the slim fluorescence liquid pool of 1～5mm * 10～30mm.
5. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 1 is characterized in that in step 3), and described front surface radiation modality is meant and allows exciting light become 20 °～40 ° or 55 °～70 ° angles with the liquid pool sensitive surface.
6. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 5 is characterized in that in step 3), and described front surface radiation modality is meant and allows exciting light become 30 ° of angle irradiation liquid pools with the liquid pool sensitive surface.
7. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 1, it is as follows to it is characterized in that described quantitative fluorescence mensuration is obtained its step of the crude oil range of linearity:
1) the permanent energy synchronous scanning of fluorospectrophotometer wave-number difference being set is 1100～1600cm
-1
2) the diluent crude oil solution for preparing is poured into respectively in the conventional liquid pool of 10mm * 10mm, allowed exciting light shine liquid pool, according to the above-mentioned parameter scanning constant-energy synchronous fluorescence spectrum that sets with vertical mode;
3) the diluent crude oil solution for preparing is poured into respectively in the slim liquid pool of 1～5mm * 10～30mm, allow the former surface based fashion of exciting light shine liquid pool, exciting light becomes 20 °～40 ° or 55 °～70 ° angles with the liquid pool sensitive surface, according to the parameter scanning constant-energy synchronous fluorescence spectrum that sets;
4) collection of illustrative plates after will scanning is preserved, and reads peak value, with data processing software match working curve.
8. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 7 is characterized in that in step 1), and the permanent energy synchronous scanning of described fluorospectrophotometer wave-number difference is 1400cm
-1
9. a kind of rationing fluorescent logging method that enlarges crude oil linear analysis scope as claimed in claim 7, it is characterized in that in step 1), the described diluent crude oil solution for preparing is poured into respectively in the slim liquid pool of 1mm * 20mm, allow the former surface based fashion of exciting light shine liquid pool, exciting light becomes 30 ° of angles with the liquid pool sensitive surface, according to the parameter scanning constant-energy synchronous fluorescence spectrum that sets.
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| US11733163B2 (en) | 2017-08-21 | 2023-08-22 | Saudi Arabian Oil Company | Determining composition of a sample |
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| US11726038B2 (en) | 2017-08-21 | 2023-08-15 | Saudi Arabian Oil Company | Determining composition of a sample |
| US11733163B2 (en) | 2017-08-21 | 2023-08-22 | Saudi Arabian Oil Company | Determining composition of a sample |
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