CN100390529C - Method for measuring oil content of debris and core in oil logging - Google Patents
Method for measuring oil content of debris and core in oil logging Download PDFInfo
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- CN100390529C CN100390529C CNB2005100020877A CN200510002087A CN100390529C CN 100390529 C CN100390529 C CN 100390529C CN B2005100020877 A CNB2005100020877 A CN B2005100020877A CN 200510002087 A CN200510002087 A CN 200510002087A CN 100390529 C CN100390529 C CN 100390529C
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Abstract
The present invention relates to a method for measuring the oil content of rock fragments and rock cores in oil wells, which comprises the steps that the wavelength difference delta lambada of the optimal synchronous scanning is selected from samples in the same oil region; the synchronous fluorescence spectra of different concentrations in the range of concentration measurement are collected by the fixed delta lambada; then the interpolation processing of data is carried out by utilizing universal mathematical processing software MATLAB to form a continuous three-dimensional concentration synchronous fluorescence spectrum database; the comparison of the spectrum data of a least square method of the synchronous spectrum of a certain concentration sample and the database is carried out, and the concentration corresponding to the spectrum data having the minimum difference value is the oil content of rock cores or rock fragments. The present invention is suitable for measuring other concentrations of various aromatic compounds or mixtures, the fluorescent effect is needed, and the corresponding solvent is selected. Therefore, the present invention is suitable for multi-component mixtures and has the advantages of simple operation, high accuracy and large concentration measurement range, such as the concentration measurement of the fluorescence spectrum of oil and the measurement of the oil content of rock fragments and rock cores in oil wells.
Description
Technical field
The present invention relates to the measuring method of landwaste core oleaginousness in a kind of oil log.
Background technology
Because oil has the characteristic of fluorescence, external sand smeller is applied to situ of drilling well the thirties in 20th century with detection technique of fluorescence, be placed on down irradiation of uviol lamp in the camera bellows to returning out landwaste in the drilling well, fluorescence phenomenon (color and rank) by visual inspection record landwaste, understanding whether oil-containing of earth cuttings, thereby judge the oil generation and the storage characteristics on stratum.The detection technique of fluorescence of this routine is still used at situ of drilling well so far, still has certain directive function in exploratory development.Along with deepening continuously of oil-gas exploration, the exploratory development object of facing becomes increasingly complex, and difficulty is also increasing; The quickening of bit speed in addition, the application of PDC drill bit, the increase of highly difficult wells such as orientation well and horizontal well, the difficulty that makes well logging find and estimate hydrocarbon zone increases, and traditional well logging technology and method can not adapt to the needs of oil-gas exploration and development fully.In view of the fluorescence spectrophotometer utensil have highly sensitive, analysis speed is fast, most of method is not destroyed sample, can combine and use a computer with the microscopic appearance analysis to analyze the reliable easily characteristics of row of spectroscopic data method.The fluorescent instrument of some oil logs of successively developing is (as the OFA quantitative fluorescence detector of explore institute of PetroChina Company Limited. research and development both at home and abroad, last sea God opens the SK-2DQF quantitative fluorescence detector of research and development etc.) it is mainly according to the relation of emission spectrum fluorescence intensity and crude oil sample concentration, and method of work is similar.But the two-dimensional quantitative data that exist in the practice are single, and accuracy is not high, and concentration determination narrow range (10
-4G/l～10
-2Problem such as g/l).
And the high-grade spectral instrument that the three-dimensional fluorescence spectrum technology will rely on be introduced, though spectral information is abundant, the collection and the data processing of spectrum are loaded down with trivial details, thereby have influenced the process that fluorescent technique becomes the main force's analysis means in the Petroleum Geology Laboratory.In addition, on data acquisition and handling, the method of OFA quantitative fluorescence detector and the analysis of SK-2DQF quantitative fluorescence detector is to adopt the single-point of two-dimentional emission spectrum quantitative, promptly determine the sample oleaginousness with the relation of concentration according to single peak value in the concentration linear response range, this single-point quantitative analysis method only is fit to one-component or each component small situation that influences each other.But oil is the multicomponent system that contains the complexity of multiple aromatic compound, and the variation of concentration not only causes the variation of spectrum peak heights, composes shape simultaneously bigger variation also takes place.As shown in Figure 1.Since have that fluorescence quenching causes non-linear add and, each component quenching concentration difference, responding range also has bigger difference.Therefore, diluted sample is not high to the single-point quantitative analysis method accuracy in the range of linearity, simultaneously also can strengthen the loaded down with trivial details of the use of experiment reagent and program because of dilution repeatedly.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of simple and direct fast, measuring accuracy is high, measurement range is big, be applicable to the measuring method of oil log measurement landwaste core oleaginousness.
Method of the present invention is at first to take by weighing the sample of a certain wellblock crude oil as concentration calibration, and it is configured to standard specimen extract in the sample concentration fluorescence range of linearity with solvent, determines the wavelength difference Δ λ of best synchronous scanning; Then above-mentioned crude oil sample is obtained the extract of variable concentrations as the concentration calibration specimen according to half-and-half dilution process progressively in the measurement of concetration scope, with above-mentioned optimal wavelength difference Δ λ, carry out the spectral measurement of synchronous fluorimetry respectively and it is carried out level and smooth and normalized again; Then above-mentioned spectroscopic data all is input to the three-dimensional synchronous fluorescent spectrum database that generates concentration among the general mathematics manipulation software MATLAB, the row interpolation of going forward side by side is handled, to form concentration continuous three-dimensional synchronous fluorescent spectrum database; When measuring the oleaginousness of a certain core to be measured or chip sample, as long as measure the synchronous two-dimensional fluorescence spectrum of the extract of this sample, and after equally smoothly reaching normalization, do the contrast one by one of least square method with the spectroscopic data in the above-mentioned database, the spectroscopic data institute corresponding concentration of difference minimum wherein promptly be can be converted into core or landwaste oleaginousness.
Common synchronous fluorescent spectrum is to scan excitation wavelength lambda at the same time
Ex MaxAnd emission wavelength lambda
Em MaxThe time keep the spectrum of fixing wavelength difference Δ λ gained between the two.For one-component, can select wavelength difference easily
The narrow fluorescence peak with regard to obtaining point.But for the such multicomponent mixture of image-stone oil, a plurality of spectral line spikes that the selection of different Δ λ can obtain.Therefore select the best Δ λ can be to greatest extent and the information of the three-dimensional spectrum of the most effective reflection.Be that one of key problem in technology is determining of wavelength difference Δ λ, the definite of Δ λ can adopt two kinds of methods, and choosing concentration usually is that (crude oil is generally 10 for the linear range limit of fluorescence
-2The g/l place) crude oil sample extract is a benchmark.
One of definite method of wavelength difference Δ λ is to have three-dimensional plot spectrometer or three-dimensional collection of illustrative plates to obtain easily under the situation, earlier the three-dimensional spectrum that the extract of the crude oil sample of this concentration is obtained contour map as shown in Figure 3, then in its contour map, choosing slope with main peak peak position and peak-to-peak maximum separation degree is that 1 the straight line and the intercept of emission wavelength Em axle are Δ λ, as shown in Figure 4.Two of method is to lack three-dimensional instrument or obtaining the method that three-dimensional collection of illustrative plates also can accurately be chosen Δ λ at need, carry out the synchronous scanning of different wave length difference for extract, measure a synchronous spectrum every identical wavelength such as 10nm in promptly in 20nm～70nm scope, choose the maximum pairing Δ λ of spectrogram the highest and peak-to-peak degree of separation maximum of main peak and be best wavelength difference Δ λ.
When the setting up of the concentration synchronous fluorescent spectrum database of standard, preferably use the method for two-dimentional cubic convolution interpolation in addition, so that 10
-4How can obtain continuous concentration three-dimensional fluorescence spectrum database through after the interpolation processing in g/l～10g/l concentration range with less spectroscopic data, the present invention utilizes two-dimentional cubic convolution interpolation algorithm to can solve the discontinuous problem of data in the concentration three-dimensional plot, has also significantly reduced the workload when database is set up.As long as this convolution interpolation algorithm utilizes the interp2 order among the general mathematics manipulation software MATLAB to realize.
Description of drawings
Fig. 1 is variable concentrations ((the interval delta λ of excitation wavelength and emission wavelength=40nm) of the two-dimentional synchronous fluorescent spectrum under the A～G) of crude oil sample of the present invention.
Fig. 2 is the oil sample synchronous fluorimetry concentration three-dimensional fluorescence database in a certain oil district that the present invention set up.
Fig. 3 is the three dimensional emission fluorescence spectrum figure of crude oil sample of the present invention.
Fig. 4 is the pairing level line perspective view of three dimensional emission fluorescence spectrum figure among Fig. 3, and slope is that the straight line of l and the intercept of emission wavelength promptly are wavelength difference Δ λ in the contour map.
Embodiment
The present invention at first need take by weighing the sample of a certain wellblock crude oil as concentration calibration, and it is dissolved in normal hexane or the isopropanol solvent, is configured to concentration 10
-2The extract of g/l can select for use two kinds of distinct methods to choose best wavelength difference Δ λ under different experiment conditions, promptly scans excitation wavelength lambda
Ex MaxAnd emission wavelength lambda
Em MaxPoor.With above-mentioned crude oil sample 1.0 * 10
-4As long as g/l in the 10g/l concentration range according to half-and-half method progressively obtain 18 successively the n-hexane extract of dilute concentration as the concentration calibration specimen.And then fixing above-mentioned optimal wavelength difference Δ λ, the employing synchronous fluorimetry is measured the spectrum of above-mentioned 18 standards respectively and spectroscopic data is carried out level and smooth and normalized, above-mentioned spectroscopic data all is input to the three-dimensional synchronous fluorescent spectrum database that generates concentration among the general mathematics manipulation software MATLAB, and utilize the interp2 order among the MATLAB that above-mentioned database is carried out two-dimentional cubic convolution interpolation, to form concentration continuous three-dimensional synchronous fluorescent spectrum database, as shown in Figure 2.When measuring the oleaginousness of a certain core to be measured or chip sample, as long as this sample is dissolved in normal hexane or the isopropyl alcohol, and measure the synchronous two-dimensional fluorescence spectrum of its extract, after this spectroscopic data smoothly reached normalization, do the contrast one by one of least square method with the spectroscopic data in the above-mentioned database, the spectroscopic data institute corresponding concentration of difference minimum promptly can be converted into core or landwaste oleaginousness.
Embodiment 1:
One, same wellblock sample is chosen the best excitation wavelength and the difference Δ λ of emission wavelength.
1, at first takes by weighing the sample of a certain wellblock crude oil as concentration calibration with electronic scales, it is dissolved in the normal hexane solvent, be configured to the crude oil standard specimen of a certain concentration value in the concentration range of linearity, inject the fluid sample pond of fluorospectrophotometer, choosing excitation wavelength begins up to 600nm from 220nm, survey an emission spectrum every 5nm, whole spectroscopic datas are input to generate three-dimensional light spectrogram and contour map among the MATLAB.
2, in three-dimensional contour map, with through the main peak peak position of three-dimensional spectrum and guarantee maximum peak-to-peak degree of separation simultaneously, choose slope and be 1 the straight line and the intercept of emission wavelength Em axle and be best Δ λ.
Two, set up normal concentration three-dimensional fluorescence spectrum database
1, the configuration of concentration: above-mentioned crude oil sample is allotted 1.0 * 10 with normal hexane as solvent
4The sample extraction liquid of g/l under the 10g/l variable concentrations is as demarcating specimen.
2, the measurement of spectrum: the extract of its each concentration is injected the fluid sample pond of fluorospectrophotometer successively, under the condition of the above-mentioned Δ λ of choose, obtain synchronous fluorescent spectrum.
3, the generation B of database: with the synchronous spectrum data normalization that is obtained, be about to each spectroscopic data divided by separately peak-peak, the data after the above-mentioned normalization be input to the synchronous fluorescence concentration three-dimensional data base that generates among the MATLLAB behind two-dimentional cubic convolution interpolation.
Three, determine the oleaginousness of testing sample:
1, spectral measurement to be measured: core to be measured or chip sample 0.025g are dissolved in the 5ml normal hexane, left standstill 30 minutes, so that the oil composition in the core, chip sample fully dissolves, this extract is placed the fluorospectrophotometer sample cell, keep recording the synchronous fluorescent spectrum of testing sample under the condition consistent with above-mentioned experiment condition.
2, spectrum identification: with after institute's photometry spectrum normalization with above-mentioned synchronous fluorescence concentration three-dimensional data base in spectroscopic data do the contrast one by one of least square method, be core or landwaste oleaginousness behind the concentration conversion of difference minimum.
Embodiment 2:
Lack three-dimensional instrument or obtaining three-dimensional fluorescence spectrum at need, when determining best Δ λ, can only rely on the Δ λ that chooses certain intervals to be two-dimensional fluorescence spectrum figure, maximum pairing Δ λ of spectrogram the highest and peak-to-peak degree of separation maximum are best Δ λ with main peak, and other steps are substantially with embodiment 1.
One, same wellblock sample is chosen the difference Δ λ of suitable excitation wavelength and emission wavelength
1, be example with a certain wellblock: normal hexane reagent can adopt chromatographically pure reagent or specpure reagent, and choosing concentration is 6.3 * 10
-2The g/l crude oil sample, successively to different scanning wavelength difference Δ λ=20nm, 30nm, 40nm, 50nm, 60nm, 70nm carry out synchronous fluorescent spectrum and measure in day island proper Tianjin RF5301 of company fluorophotometer.
2, comparing result is selected best Δ λ: in the spectrum that obtains, choose the main peak pairing Δ λ of spectrogram the highest and peak-to-peak degree of separation maximum at most.Determine optimum scanning wavelength difference Δ λ=40nm at last.
Two, set up normal concentration three-dimensional fluorescence spectrum database
1, the configuration of concentration: above-mentioned primary sample is allotted 1.0 * 10 with normal hexane as solvent
-4The sample extraction liquid of g/l under the 10g/l variable concentrations is as demarcating specimen.
2, the measurement of spectrum: the extract of its each concentration is injected the fluid sample pond of fluorospectrophotometer successively, measure 10
-4The synchronous fluorescent spectrum of Δ λ=40nm in g/l～10g/l concentration range.
3, these spectroscopic datas are generated the three-dimensional synchronous fluorescence collection of illustrative plates of concentration with MATLAB, three coordinate axis XYZ are respectively: the logarithm value X=log of concentration
22
13C, emission wavelength and fluorescence intensity, as shown in Figure 2.And the method for specialized application two dimension cubic convolution interpolation forms continuous concentration three-dimensional fluorescence collection of illustrative plates.Set up a measurement range thus from 10
-4The three-dimensional synchronous fluorescent spectrum database of the concentration of Δ λ=40nm of g/l～10g/l.
Three, determine the oleaginousness of testing sample:
1, the spectral measurement of testing sample: core to be measured or chip sample 0.025g are dissolved in the 5ml normal hexane, left standstill 30 minutes, so that the oil composition in the core, chip sample fully dissolves, this extract is statically placed in fluorospectrophotometer, keep the experiment condition unanimity, record synchronous fluorescent spectrum.
2, determine oleaginousness: with after the normalization of testing sample spectrum with the three-dimensional synchronous fluorimetry database of concentration in data do the contrast one by one of least square method, be core or landwaste oleaginousness behind the concentration conversion of difference minimum.
In addition, consider that concentration range is bigger, the configuration solution of setting up the concentration calibration database for minimizing is loaded down with trivial details, only need obtain 18 concentration of dilution successively according to half-and-half method progressively in the sample preparation layoutprocedure; Consider the accuracy in the measurement, before each replacing sample, with normal hexane sample cell is cleaned, and carry out normal hexane background spectral detection in the experiment to guarantee that no remaining sample is residual in the pond.
In sum, it is normal hexane or isopropyl alcohol that the present invention adopts the solvent of crude oil sample, and this method is applicable to that also other contains the measurement of concetration of multiple aromatic compound or potpourri in principle, as long as select corresponding solvent.Therefore the present invention is more suitable in multicomponent mixture and to measure concentration range big, and the instant measurement of landwaste and core oleaginousness is simple to operate in measurement of concetration, the especially oil log of the fluorescence spectrum of image-stone oil one class, the accuracy height.
Claims (7)
1. the measuring method of landwaste core oleaginousness in the oil log, it is characterized in that at first taking by weighing the sample of a certain wellblock crude oil as concentration calibration, it is configured to standard specimen extract in the sample concentration fluorescence range of linearity with solvent, determine the wavelength difference Δ λ of best synchronous scanning, then above-mentioned crude oil sample is obtained the extract of variable concentrations as the concentration calibration specimen according to half-and-half dilution process progressively in the measurement of concetration scope, with the synchronous scanning wavelength difference Δ λ of above-mentioned the best, carry out the spectral measurement of synchronous fluorimetry respectively and it is carried out level and smooth and normalized again; Then spectroscopic data all is input to the three-dimensional synchronous fluorescent spectrum database that generates concentration among the general mathematics manipulation software MATLAB, and adopt the data processing method of three convolution of two dimension to carry out interpolation processing, to form concentration continuous three-dimensional synchronous fluorescent spectrum database; When measuring the oleaginousness of a certain core to be measured or chip sample, as long as measure the synchronous two-dimensional fluorescence spectrum of the extract of this sample, and after equally smoothly reaching normalized, do the contrast one by one of least square method with the spectroscopic data in the above-mentioned database, will be converted into core or landwaste oleaginousness with the spectroscopic data institute corresponding concentration of testing sample experiment institute photometry spectral difference value minimum in the database.
2. the measuring method of landwaste core oleaginousness in the oil log according to claim 1, the method that it is characterized in that the synchronous scanning wavelength difference Δ λ of above-mentioned definite the best, be the three-dimensional spectrum that earlier extract of crude oil sample concentration in the fluorescence range of linearity is obtained contour map, then in its contour map, choosing slope with main peak peak position and peak-to-peak maximum separation degree is that 1 the straight line and the intercept of emission wavelength Em axle are optimal wavelength difference Δ λ.
3. the measuring method of landwaste core oleaginousness in the oil log according to claim 1, the method that it is characterized in that the synchronous scanning wavelength difference Δ λ of above-mentioned definite the best, be earlier crude oil sample to be configured to standard specimen extract in the sample concentration fluorescence range of linearity with solvent, and extract is carried out the synchronous scanning of different wave length difference Δ λ, in 20nm～70nm scope, measure a synchronous spectrum, choose the maximum pairing Δ λ of spectrogram the highest and peak-to-peak degree of separation maximum of main peak wherein every 10nm.
4. according to the measuring method of landwaste core oleaginousness in claim 1 or the 2 or 3 described oil logs, the data processing method that it is characterized in that the two-dimentional cubic convolution interpolation in the above-mentioned interpolation processing is to utilize the interp2 order among the general mathematics manipulation software MATLAB to realize.
5. according to the measuring method of landwaste core oleaginousness in claim 1 or the 2 or 3 described oil logs, the concentration that it is characterized in that above-mentioned standard specimen extract is 10
-2G/l.
6. the measuring method of landwaste core oleaginousness in the oil log according to claim 1 is characterized in that the measurement of concetration scope of above-mentioned crude oil sample is 1.0 * 10
-4G/l is in the 10g/l scope.
7. the measuring method of landwaste core oleaginousness in the oil log according to claim 1 is characterized in that above-mentioned solvent is normal hexane or isopropyl alcohol reagent.
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| CN101566569B (en) * | 2009-04-30 | 2011-09-14 | 西南科技大学 | System and method for identifying a plurality of fluorescence spectrum mixed materials through characteristic parameter |
| CN102128817A (en) * | 2010-12-09 | 2011-07-20 | 中国石油集团川庆钻探工程有限公司长庆录井公司 | Three-dimensional quantitative fluorescence spectrum total volume integral method |
| CN104076019B (en) * | 2014-07-22 | 2016-11-23 | 中国海洋石油总公司 | A kind of method utilizing 3-D quantitative fluorescence measurement parameter to judge oil type |
| CN104100262A (en) * | 2014-07-22 | 2014-10-15 | 中国海洋石油总公司 | Method for identifying properties of reservoir fluid by three-dimensional quantitative fluorescence parameter charts |
| CN105987925B (en) * | 2015-02-28 | 2018-05-08 | 中国石油化工股份有限公司 | The oil content of oil-based drill cuttings and/or the measuring method of oil content and its application |
| CN110658162B (en) * | 2018-06-29 | 2022-03-11 | 中国石油化工股份有限公司 | Method for predicting crude oil concentration in rock debris extraction liquid by three-dimensional fluorescence spectrum |
| CN110836878B (en) * | 2019-11-01 | 2021-09-07 | 同济大学 | Convolution interpolation coupling Gaussian mixture model rapid three-dimensional fluorescence peak searching method |
| CN113125616A (en) * | 2019-12-30 | 2021-07-16 | 中石化石油工程技术服务有限公司 | Two-dimensional chromatographic logging analysis device and method |
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