# US 2019/0170644 A1 · Method for determining maturity in oil source rock by total scanning fluorescence and the device therefor

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- Number: US 2019/0170644 A1
- Document ID: US20190170644A1
- Status: Published application
- Kind: A1
- Application number: 16/170,914
- Filed: 2018-10-25
- Published: 2019-06-06
- Earliest claimed: 2017-10-27
- Assignees: PetroChina Company Limited
- Applicants: PetroChina Company Limited
- Inventors: Keyu LIU; Hua TIAN; Caineng ZOU; Shuichang ZHANG; Shaobo LIU; Mengjun ZHAO; Xuesong LU; Junjia FAN; Xiuli LI; Lili GUI; Qingong ZHUO; Xingzhi MA; Yanjie GONG; Zhichao YU; Qingyang MENG
- Web page: https://patentgrep.com/patent/US20190170644A1

## CPC

- G01N 21/645: {Specially adapted constructive features of fluorimeters}
- G01J 3/4406: {Fluorescence spectrometry}
- G01N 21/643: {non-biological material}
- G01N 33/2823: {Raw oil, drilling fluid or polyphasic mixtures}
- G01N 2021/6417: {Spectrofluorimetric devices}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- G01J: MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY (light sources F21, H01J, H01K, H05B; investigating properties of materials by optical means G01N)

## Abstract

A device and method of determining thermal maturity of oil source rocks by total scanning fluorescence including testing the organic solution of the extract from a series of oil source rock samples collected at different depths by total scanning fluorescence; building a model for interpretation of the oil source rock maturity according to the variation with depth of the TSF Intensity parameter and the TSF R1 parameter obtained by total scanning fluorescence, and identifying the stage of initial oil generation, the stage of major oil generation and the stage of major gas generation; and establishing the relationship between the TSF Intensity parameter and/or the TSF R1 parameter with the existing characteristic parameters that quantitatively characterize the maturity of oil source rocks, thereby accomplishing the analysis and determination of the maturity of the oil source rocks.

## Claims

### Claim 1

A method of determining thermal maturity of oil source rocks by total scanning fluorescence, the method comprising:
testing the organic solution of an extract from a series of oil source rock samples collected at different depths by total scanning fluorescence, wherein a concentration of the extract in the organic solution is 0.01 ppm to 1000 ppm; and obtaining TSF Intensity parameters and TSF R1 parameters of the fluorescence spectrum, wherein the TSF Intensity is the value of the maximum fluorescence intensity in the total scanning fluorescence spectrum, and the TSF R1 is the ratio of the intensity at 360 nm to the intensity at 320 nm of the fluorescence spectrum with an emitting light at 270 nm;
building a model for interpretation of the oil source rock maturity according to the variation with depth of the TSF Intensity parameter and the TSF R1 parameter obtained by total scanning fluorescence, and identifying the stage of initial oil generation, the stage of major oil generation and the stage of major gas generation; wherein the identification criterion lies in that the initial position of the stage of initial oil generation is set when the increase of the TSF R1 parameter becomes leveling, the initial position of the stage of major oil generation is set when the TSF R1 parameter turns from leveling to decreasing, and the initial position of the stage of major gas generation is set when the TSF Intensity parameter turns from leveling to decreasing; and
establishing the relationship between the TSF Intensity parameter and/or the TSF R1 parameter with existing characteristic parameters that quantitatively characterize the maturity of oil source rocks, thereby accomplishing the analysis and determination of the maturity of the oil source rocks.

### Claim 2 (depends on 1)

The method of claim 1, wherein the concentration of the extract in the organic solution is 1 ppm to 100 ppm.

### Claim 3 (depends on 1)

The method of claim 1, wherein establishing the relationship between the TSF Intensity parameter and/or the TSF R1 parameter with the existing characteristic parameters for quantitatively characterize the maturity of oil source rocks comprises establishing a calibration curve of the TSF Intensity parameter and/or the TSF R1 parameter restricted by the existing characteristic parameters that quantitatively characterize the maturity of the oil source rocks.

### Claim 4 (depends on 3)

The method of claim 3, further comprising establishing a database of calibration curves from different regions so that TSF R1 is directly used as the indication of maturity.

### Claim 5 (depends on 1)

The method of claim 1, wherein the existing characteristic parameters that quantitatively characterize the maturity of oil source rocks include vitrinite reflectance, rock pyrolysis, the degree of spore-pollen carbonization, or thermal alteration index.

### Claim 6 (depends on 1)

The method of claim 1, wherein the existing characteristic parameter that quantitatively characterizes the maturity of the oil source rocks is vitrinite reflectance.

### Claim 7 (depends on 1)

The method of claim 1, wherein the process of preparing the organic solution of the extract comprises pulverizing the sample to be tested with the mass of Mr, adding the organic solvent, and ultrasonically extracting at least twice; and diluting to the preset concentration after extraction to prepare the organic solution of the extract.

### Claim 8 (depends on 7)

The method of claim 7, wherein the process of preparing the organic solution of the extract comprises:
obtaining an uncontaminated sample from the sample to be tested, and pulverizing the sample particles to a certain particle size;
selecting a rock sample to be measured with the mass of Mr, adding 10 mL organic solvent, and ultrasonically extracting for 10 minutes, wherein Mr is in the range of 0.1 g-1.0 g;
standing for 10 minutes, and further ultrasonically extracting for 10 minutes;
standing for a certain period of time, and transferring Vl mL into an analysis dish, into which 3 mL of the organic solvent is added, wherein Vl is in the range of 0.001 mL-0.1 mL; and
placing the analysis dish in a fluorescence spectrometer for testing, measuring the TSF Intensity original parameter and TSF R1 parameter of the fluorescence spectrum, and correcting the TSF Intensity original parameter by multiplying by 0.1*3/(Mr*Vl) to obtain the TSF Intensity parameter.

### Claim 9

A device for determining thermal maturity of oil source rocks by total scanning fluorescence, the device comprising:
a first unit for testing by total scanning fluorescence, an organic solution of the extract of a series of oil source rock samples collected at different depths, wherein, the concentration of the extract in the organic solution is 0.01 ppm to 1000 ppm; thus obtaining the TSF Intensity parameter and TSF R1 parameter of the total scanning fluorescence spectrum, wherein the TSF Intensity is the value of the maximum fluorescence intensity in the total scanning fluorescence spectrum, and the TSF R1 is the ratio of the intensity of the fluorescence spectrum at 360 nm to the intensity of 320 nm with an emitting light at 270 nm;
a second unit for building a model for interpretation of the oil source rock maturity according to the variation with depth of the TSF Intensity parameter and the TSF R1 parameter obtained by total scanning fluorescence, and identifying the stage of initial oil generation, the stage of major oil generation and the stage of major gas generation; wherein the identification criterion lies in that the initial position of the stage of initial oil generation is set when the increase of the TSF R1 parameter becomes leveling, the initial position of the stage of major oil generation is set when the TSF R1 parameter turns from leveling to decreasing, and the initial position of the stage of major gas generation is set when the TSF Intensity parameter turns from leveling to decreasing; and
a third unit for establishing the relationship between the TSF Intensity parameter and/or the TSF R1 parameter with existing characteristic parameters that quantitatively characterize the maturity of oil source rocks, thereby accomplishing the analysis and determination of the maturity of the oil source rocks.

### Claim 10 (depends on 9)

The device of claim 9, wherein the concentration of the extract in the organic solution is 1 ppm to 100 ppm.

### Claim 11 (depends on 9)

The device of claim 9, wherein, in the third unit, the process of establishing the relationship between the TSF Intensity parameter and/or the TSF R1 parameter with the existing characteristic parameters that quantitatively characterize the maturity of oil source rocks comprises establishing a calibration curve of the TSF Intensity parameter and/or the TSF R1 parameter restricted by the existing characteristic parameters that quantitatively characterize the maturity of the oil source rocks.

### Claim 12 (depends on 9)

The device of claim 9, further comprising a fourth unit for establishing a database of calibration curves from different regions so that TSF R1 is directly used as the indication of maturity.