CN111157648A - Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample - Google Patents

Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample Download PDF

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CN111157648A
CN111157648A CN202010008574.9A CN202010008574A CN111157648A CN 111157648 A CN111157648 A CN 111157648A CN 202010008574 A CN202010008574 A CN 202010008574A CN 111157648 A CN111157648 A CN 111157648A
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crude oil
sample
analysis
standard substance
gas chromatography
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金洪蕊
李政
王�忠
鲍燕
王茹
刘旋
宋长玉
邸晓君
任英姿
曹智
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8675Evaluation, i.e. decoding of the signal into analytical information
    • G01N30/8679Target compound analysis, i.e. whereby a limited number of peaks is analysed
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
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Abstract

The invention relates to the technical field of oil field exploration and development, in particular to a rapid quantitative analysis method for saturated hydrocarbon gas chromatography in a crude oil sample. The method comprises the following steps of 1, preparing a standard substance solution; step 2, weighing a proper amount of crude oil sample; step 3, adding a standard sample and a reagent into the crude oil sample to obtain a crude oil detection solution; step 4, filling the crude oil detection solution into a sample bottle, and putting the sample bottle into an ultrasonic cleaner for uniformly mixing by oscillating; step 5, placing the sample bottle into a centrifuge for centrifugal separation; and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution, and carrying out quantitative analysis. The crude oil sample can be subjected to chromatographic analysis without being treated by a chromatographic column, so that the operation steps are simplified, the reagent dosage is reduced, the analysis process is shortened, and the analysis data can be quickly provided.

Description

Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample
Technical Field
The invention relates to the technical field of oil field exploration and development, in particular to a rapid quantitative analysis method for saturated hydrocarbon gas chromatography in a crude oil sample.
Background
Along with the development of industry, the requirement of human beings on energy is sharply increased, crude oil and products thereof become the most important energy at present, and along with the continuous exploration and development of petroleum in recent years, the phenomena of crude oil running, overflowing, dripping and leaking caused by factors such as exploitation, transportation, various oil pipeline aging and perforation and the like occur for many times. Once oil spill occurs, due to the lack of systematic and comprehensive oil spill identification basis and a quick and effective oil spill identification method, the identification of the crude oil source usually costs a great deal of manpower and material resources, and the oil spill point is determined quickly and in time with great difficulty, so that the pollution is continuously expanded; meanwhile, the responsibility units of the pollution events cannot be checked in time, the pollution events cannot be processed in time, the environment is polluted, huge economic loss is caused, and the normal production order of enterprises is influenced due to long-time pollution disputes. Therefore, after oil spill occurs on land or at sea, timely and correct judgment of oil pollution sources is an important basis for quickly finding oil spill points, determining environmental responsibility and solving responsibility disputes, and is also necessary work for quickly making appropriate countermeasures, effectively clearing methods and accurately predicting long-term risks.
The main part of petroleum is hydrocarbons, which can account for more than 75% of petroleum fractions, and the content of normal paraffin and isoprenoid in the hydrocarbons is controlled by the original organic matter property, thermal evolution degree, biodegradation and other factors, so that the analysis and test data of the substances is one of important bases for oil and gas source research in the oil and gas exploration process. The currently used analysis method is that according to SY/T5119-2008, after a sample passes through a chromatographic column and is separated to obtain a saturated hydrocarbon component, chromatographic analysis can be carried out. Aiming at the emergency, the method has the defects of long analysis period, incapability of providing analysis data in time and insufficient analysis data.
Therefore, it is highly desirable to provide a new method for rapid gas chromatography quantitative analysis of saturated hydrocarbons in crude oil samples. The technical problem is solved.
Disclosure of Invention
In order to solve the problems, the invention provides a rapid quantitative analysis method for saturated hydrocarbon gas chromatography in a crude oil sample, which can rapidly analyze saturated hydrocarbon series normal paraffin and isoprenoid in crude oil and is convenient for providing analysis data in time.
The purpose of the invention can be realized by the following technical scheme:
a method for rapid gas chromatographic quantitative analysis of saturated hydrocarbons in a crude oil sample, the method comprising the steps of:
step 1, preparing a standard substance solution;
step 2, weighing a proper amount of crude oil sample;
step 3, adding a standard sample and a reagent into the crude oil sample to obtain a crude oil detection solution;
step 4, filling the crude oil detection solution into a sample bottle, and putting the sample bottle into an ultrasonic cleaner for uniformly mixing by oscillating;
step 5, placing the sample bottle into a centrifuge for centrifugal separation;
and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution, and carrying out quantitative analysis.
The purpose of the invention can be realized by the following technical scheme:
in the step 1, deuterated tetracosane is used as a standard substance, and isooctane is used as a solvent;
preferably, the concentration of the standard substance solution is 200. mu.g/mL.
Weighing 15-20mg of crude oil sample in the step 2; preferably, the crude oil sample is 18 mg.
In step 3, 50-100 μ L of standard solution is added to the crude oil sample, and the volume is adjusted to 1mL by using isooctane, so as to obtain the crude oil detection solution.
In step 4, ultrasonic treatment is carried out in an ultrasonic cleaner for 10-15 min.
In step 5, centrifugation is carried out at 3000-5000r/min for 5-10 min.
In step 6, an HP5 capillary chromatography column was used, with a specification of 30m by 0.25mm by 0.25 μm.
The chromatographic analysis conditions in the step 6 are as follows:
temperature: the initial temperature is 60 ℃, after staying for 2min, the temperature is raised to 300 ℃ by a program of 5 ℃/min, and the temperature is kept for 30 min;
carrier gas: high-purity nitrogen;
flow rate: 1.0mL/min, split mode: no flow diversion;
sample inlet temperature 300 ℃, sample injection amount: 1 μ L.
In step 6, the concentration Cn (μ g/g) of each compound in the sample is calculated by the formula:
Cn=(Sn*CS)/SS
in the formula, SSIs the peak area of the standard substance, CSSn is the peak area of the compound as the concentration of the standard substance.
The invention has the following beneficial effects:
according to the rapid quantitative analysis method for the gas chromatography of the saturated hydrocarbon in the crude oil sample, on one hand, the crude oil sample can be subjected to chromatographic analysis without being treated by a chromatographic column, so that the operation steps are simplified, the reagent dosage is reduced, the analysis time is shortened, and the analysis data can be rapidly provided; on the other hand, the addition of the internal standard can carry out quantitative calculation on each compound in the sample to obtain the absolute content of each compound, and richer analysis data can be provided.
Drawings
FIG. 1 is a flow chart of an embodiment of a method for rapid gas chromatography quantitative analysis of saturated hydrocarbons in a crude oil sample according to the present invention;
FIG. 2 is a series of chromatograms of normal alkanes from gas chromatography in an embodiment of the present invention;
FIG. 3 is a chromatogram of isoprenoid from a gas chromatography analysis in an embodiment of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1 gas chromatography rapid quantitative analysis method for saturated hydrocarbons in crude oil sample
The method comprises the following steps:
step 1, preparing a standard substance solution: preparing a standard substance solution with the concentration of 200 mu g/mL by using deuterated tetracosane as a standard substance and isooctane as a solvent;
step 2, weighing 17.60mg of a crude oil sample;
step 3, adding 100 mu L of standard solution into the crude oil sample, and diluting the volume to 1mL by using isooctane to obtain a crude oil detection solution;
step 4, filling the crude oil detection solution into a sample bottle, putting the sample bottle into an ultrasonic cleaner for ultrasonic treatment for 15min, and uniformly mixing the sample bottle with the ultrasonic cleaner;
step 5, placing the sample bottle into a centrifuge for centrifugal separation, and centrifuging for 10min at 4000 r/min;
and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution:
a chromatographic column: an HP5 capillary chromatographic column with the specification of 30m 0.25mm 0.25 μm is adopted;
the chromatographic analysis conditions were:
temperature: the initial temperature is 60 ℃, after staying for 2min, the temperature is raised to 300 ℃ by a program of 5 ℃/min, and the temperature is kept for 30 min;
carrier gas: high-purity nitrogen;
flow rate: 1.0mL/min, split mode: no flow diversion;
sample inlet temperature 300 ℃, sample injection amount: 1 μ L.
And (3) carrying out quantitative analysis according to the gas chromatographic analysis result:
the concentration Cn (. mu.g/g) of each compound in the sample was calculated by the formula:
Cn=(Sn*CS)/SS
in the formula, SSIs the peak area of the standard substance, CSSn is the peak area of the compound as the concentration of the standard substance.
Example 2 gas chromatography rapid quantitative analysis method for saturated hydrocarbons in crude oil sample
The method comprises the following steps:
step 1, preparing a standard substance solution: preparing a standard substance solution with the concentration of 200 mu g/mL by using deuterated tetracosane as a standard substance and isooctane as a solvent;
step 2, weighing 20mg of crude oil sample;
step 3, adding 50 mu L of standard solution into the crude oil sample, and diluting the volume to 1mL by using isooctane to obtain a crude oil detection solution;
step 4, filling the crude oil detection solution into a sample bottle, putting the sample bottle into an ultrasonic cleaner for ultrasonic treatment for 10min, and uniformly mixing the sample bottle with the ultrasonic cleaner;
step 5, placing the sample bottle into a centrifuge for centrifugal separation, and centrifuging for 5min at 5000 r/min;
and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution:
a chromatographic column: an HP5 capillary chromatographic column with the specification of 30m 0.25mm 0.25 μm is adopted;
the chromatographic analysis conditions were:
temperature: the initial temperature is 60 ℃, after staying for 2min, the temperature is raised to 300 ℃ by a program of 5 ℃/min, and the temperature is kept for 30 min;
carrier gas: high-purity nitrogen;
flow rate: 1.0mL/min, split mode: no flow diversion;
sample inlet temperature 300 ℃, sample injection amount: 1 μ L.
And (3) carrying out quantitative analysis according to the gas chromatographic analysis result:
the concentration Cn (. mu.g/g) of each compound in the sample was calculated by the formula:
Cn=(Sn*CS)/SS
in the formula, SSIs the peak area of the standard substance, CSSn is the peak area of the compound as the concentration of the standard substance.
Example 3 gas chromatography fast quantitative analysis method of saturated hydrocarbons in crude oil sample
The method comprises the following steps:
step 1, preparing a standard substance solution: preparing a standard substance solution with the concentration of 200 mu g/mL by using deuterated tetracosane as a standard substance and isooctane as a solvent;
step 2, weighing 15mg of a crude oil sample;
step 3, adding 100 mu L of standard solution into the crude oil sample, and diluting the volume to 1mL by using isooctane to obtain a crude oil detection solution;
step 4, filling the crude oil detection solution into a sample bottle, putting the sample bottle into an ultrasonic cleaner for ultrasonic treatment for 15min, and uniformly mixing the sample bottle with the ultrasonic cleaner;
step 5, placing the sample bottle into a centrifuge for centrifugal separation, and centrifuging for 10min at 3000 r/min;
and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution:
a chromatographic column: an HP5 capillary chromatographic column with the specification of 30m 0.25mm 0.25 μm is adopted;
the chromatographic analysis conditions were:
temperature: the initial temperature is 60 ℃, after staying for 2min, the temperature is raised to 300 ℃ by a program of 5 ℃/min, and the temperature is kept for 30 min;
carrier gas: high-purity nitrogen;
flow rate: 1.0mL/min, split mode: no flow diversion;
sample inlet temperature 300 ℃, sample injection amount: 1 μ L.
And (3) carrying out quantitative analysis according to the gas chromatographic analysis result:
the concentration Cn (. mu.g/g) of each compound in the sample was calculated by the formula:
Cn=(Sn*CS)/SS
in the formula, SSIs the peak area of the standard substance, CSSn is the peak area of the compound as the concentration of the standard substance.
Application example
Taking a crude oil sample of a well in a Shandong Shengli oil area as an example, according to the method described in example 1, 17.60mg of the sample is weighed, 100 mu L of prepared deuterated tetracosane (with the concentration of 198 mu g/mL) is added, the volume is adjusted to 1mL by isooctane, ultrasonic oscillation is carried out, separation is carried out by a centrifuge, and detection is carried out on a machine. The specific flow is shown in FIG. 1, and the obtained gas chromatogram is shown in FIGS. 1 and 2.
FIG. 2 is a chromatogram of the series of normal paraffins in the crude oil sample, and it can be seen from FIG. 2 that the series of normal paraffins in the crude oil sample can be detected according to the gas chromatography analysis method of SY/T5779-.
FIG. 3 is a chromatogram of isoprenoid in a crude oil sample, and it can be seen from FIG. 3 that pristane (Pr) and phytane (Ph) in isoprenoid series can be detected according to a gas chromatography method of SY/T5779-.
Each component detected in the sample was quantitatively analyzed, and the concentration of each compound is shown in table 1 below.
TABLE 1
Figure BDA0002354375480000051
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (9)

1. A method for quickly and quantitatively analyzing saturated hydrocarbon in a crude oil sample by gas chromatography is characterized by comprising the following steps:
step 1, preparing a standard substance solution;
step 2, weighing a proper amount of crude oil sample;
step 3, adding a standard sample and a reagent into the crude oil sample to obtain a crude oil detection solution;
step 4, filling the crude oil detection solution into a sample bottle, and putting the sample bottle into an ultrasonic cleaner for uniformly mixing by oscillating;
step 5, placing the sample bottle into a centrifuge for centrifugal separation;
and 6, carrying out gas chromatography analysis on the centrifugally separated crude oil detection solution, and carrying out quantitative analysis.
2. The method of claim 1, wherein in step 1, deuterated tetracosane is used as a standard substance, and isooctane is used as a solvent;
preferably, the concentration of the standard substance solution is 200. mu.g/mL.
3. The analytical method of claim 1, wherein 15 to 20mg of the crude oil sample is weighed in step 2.
4. The analysis method as claimed in claim 1, wherein in step 3, 50-100 μ L of the standard solution is added to the crude oil sample, and the volume is reduced to 1mL with isooctane to obtain the crude oil detection solution.
5. The method of claim 1, wherein in step 4, the sample is sonicated in a sonicator for 10-15 min.
6. The assay method according to claim 1, wherein in step 5, centrifugation is carried out at 3000-5000r/min for 5-10 min.
7. The assay of claim 1, wherein in step 6, an HP5 capillary chromatography column is used, with a specification of 30m x 0.25mm x 0.25 μm.
8. The analytical method according to claim 1, wherein the chromatographic conditions in step 6 are as follows:
temperature: the initial temperature is 60 ℃, after staying for 2min, the temperature is raised to 300 ℃ by a program of 5 ℃/min, and the temperature is kept for 30 min;
carrier gas: high-purity nitrogen;
flow rate: 1.0mL/min, split mode: no flow diversion;
sample inlet temperature 300 ℃, sample injection amount: 1 μ L.
9. The analytical method according to claim 1, wherein in step 6, the concentration Cn (μ g/g) of each compound in the sample is calculated by the formula:
Cn=(Sn*CS)/SS
in the formula, SSIs the peak area of the standard substance, CSSn is the peak area of the compound as the concentration of the standard substance.
CN202010008574.9A 2020-01-03 2020-01-03 Rapid quantitative analysis method for saturated hydrocarbon gas chromatography in crude oil sample Pending CN111157648A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN113960209A (en) * 2021-10-28 2022-01-21 中国石油天然气股份有限公司 Heavy-heavy oil gas chromatography sample introduction auxiliary device and detection method
CN114965792A (en) * 2022-06-14 2022-08-30 宁夏滨泽新能源科技有限公司 Analysis method for rapidly detecting content of C4-C22 alkane

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CN113960209A (en) * 2021-10-28 2022-01-21 中国石油天然气股份有限公司 Heavy-heavy oil gas chromatography sample introduction auxiliary device and detection method
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CN114965792A (en) * 2022-06-14 2022-08-30 宁夏滨泽新能源科技有限公司 Analysis method for rapidly detecting content of C4-C22 alkane

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Application publication date: 20200515