Analysis and detection method and device for light components in residual oil, electronic equipment and storage medium
By combining a purge-and-trap sampler and a trap with gas chromatography-mass spectrometry, the problems of easy volatility loss of light components in residual oil and instrument contamination have been solved. This has enabled efficient separation and accurate analysis of light components in residual oil, and provided a method for gaining a deeper understanding of the chemical composition of residual oil.
Patent Information
- Application Number
- CN202510148963.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-11
- Publication Date
- 2025-11-21
AI Technical Summary
Existing technologies for the analysis and detection of light components in residual oil suffer from problems such as easy loss of light components due to volatility and instrument contamination, and cannot meet the technical requirements for chemical composition research.
A purge-and-trap sampler and a trap combined with gas chromatography-mass spectrometry (GC-MS) were used to separate light components from residual oil. The light components were then efficiently captured by the trap and subsequently desorbed into the GC-MS instrument for qualitative analysis.
It reduces the loss and contamination of light components during the transfer process, achieves efficient separation and accurate analysis of light components, and provides important evidence for the chemical composition of residual oil.
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Figure CN120992782A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of petroleum composition analysis technology, and in particular to a method, apparatus, electronic device and storage medium for the analysis and detection of light components in residual oil. Background Technology
[0002] With the rapid development of the global economy, the supply of crude oil has continued to rise. However, conventional oil resources are becoming increasingly scarce, and the supply of crude oil is gradually shifting towards heavier and lower quality, resulting in a large amount of residual oil being generated during the crude oil processing process.
[0003] Currently, residual oil is mainly processed and utilized through technologies such as delayed coking and residual oil hydrogenation, and is widely used in the production of needle coke and road asphalt blending components. However, light components are generated during processing, which have potential impacts on road asphalt odor, the formation of harmful substances in waste lubricating oil, fuel oil storage and transportation safety, and the migration of heavy oil. Currently, the analysis and detection of light components in residual oil typically employs pretreatment techniques such as extraction, separation, and four-component separation combined with gas chromatography-mass spectrometry. However, this method has serious drawbacks, easily leading to the volatilization loss of light components and contaminating the instrument, failing to meet the technical requirements for studying the chemical composition of residual oil. Therefore, there is an urgent need to develop a novel analytical method for light components in residual oil. Summary of the Invention
[0004] This invention provides a method, apparatus, electronic device, and storage medium for the analysis and detection of light components in residual oil, thereby eliminating the need for pretreatment processes such as separation and extraction, reducing the loss of light components, and avoiding contamination of the gas chromatography-mass spectrometry inlet, thus effectively realizing the analysis of light components in residual oil.
[0005] In a first aspect, embodiments of the present invention provide a method for analyzing and detecting light components in residual oil, the method comprising:
[0006] The residual oil sample to be tested is purged in the purge trap sampler, and the light components purged from the residual oil sample are collected by the trap.
[0007] The light components in the residual oil sample to be tested, captured by the trap, are desorbed and introduced into a gas chromatography-mass spectrometry instrument.
[0008] Gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample.
[0009] Secondly, embodiments of the present invention also provide an analytical detection device for light components in residual oil, the device comprising:
[0010] The purge and trap module is used to purge the residual oil sample to be tested in the purge and trap sampler and to capture the light components purged from the residual oil sample through the trap.
[0011] The desorption module is used to desorb the light components in the residual oil sample to be tested captured by the trap and introduce them into the gas chromatography-mass spectrometry instrument.
[0012] The analysis and detection module is used to perform qualitative analysis and detection of light components in the desorbed residual oil sample using gas chromatography-mass spectrometry.
[0013] Thirdly, this invention also provides an electronic device, the electronic device comprising:
[0014] At least one processor; and
[0015] A memory communicatively connected to the at least one processor; wherein,
[0016] The memory stores a computer program that can be executed by the at least one processor, which enables the at least one processor to perform the analytical detection method for light components in residual oil as described in any of the above embodiments.
[0017] Fourthly, this invention also provides a computer-readable medium storing computer instructions that, when executed by a processor, implement the method for analyzing and detecting light components in residual oil as described in any of the above embodiments.
[0018] The technical solution of this invention addresses the challenge of separating highly volatile light components from a complex matrix in residual oil. Traditional methods struggle to effectively separate these components. By using a purge-and-trap sampler to purge the residual oil sample, the flow of gas can separate these components from the complex matrix. Furthermore, the use of a trap ensures efficient capture of the purged light components, even those present in extremely low concentrations. The captured light components are then desorbed and directly introduced into a gas chromatography-mass spectrometry (GC-MS) instrument. This reduces loss and contamination of light components during transfer. GC then separates the desorbed mixture of light components based on their partition coefficients between the stationary and mobile phases, allowing each component to sequentially enter the mass spectrometer. This enables accurate identification of various compounds within the light components. Qualitative analysis of the light components in the residual oil provides a deeper understanding of its chemical composition, offering crucial information for its processing and utilization.
[0019] It should be understood that the description in this section is not intended to identify key or essential features of the embodiments of the present invention, nor is it intended to limit the scope of the invention. Other features of the invention will become readily apparent from the following description. Attached Figure Description
[0020] The above and other features, advantages, and aspects of the various embodiments of the present invention will become more apparent from the accompanying drawings and the following detailed description. Throughout the drawings, the same or similar reference numerals denote the same or similar elements. It should be understood that the drawings are schematic, and the originals and elements are not necessarily drawn to scale.
[0021] Figure 1 This is a schematic flowchart of an analytical detection method for light components in residual oil provided in an embodiment of the present invention;
[0022] Figure 2 The total ion chromatogram and the extracted ion chromatogram at m / z 85 of the light components in heavy oil after purge-and-trap combined with gas chromatography-mass spectrometry analysis are shown.
[0023] Figure 3 The total ion chromatogram and the extracted ion chromatogram at m / z 85 are shown for the light components in heavy oil after purge-trap combined with gas chromatography-mass spectrometry analysis.
[0024] Figure 4 The total ion chromatogram and the extracted ion chromatogram at m / z 85 are shown for the light components in heavy oil after purge-trap combined with gas chromatography-mass spectrometry analysis.
[0025] Figure 5 The total ion chromatogram of light components in oil slurry after purge-and-trap combined with gas chromatography-mass spectrometry analysis;
[0026] Figure 6 The total ion chromatogram and extracted ion chromatogram at m / z 85 of the light components in fuel oil after purge-and-trap combined with gas chromatography-mass spectrometry analysis are shown.
[0027] Figure 7 Total ion chromatogram and extract ion chromatogram at m / z 85 of light components in coking wax oil after purge-trap combined with gas chromatography-mass spectrometry analysis;
[0028] Figure 8 Total ion chromatogram and extracted ion chromatogram at m / z 85 of light components in waste lubricating oil after purge-and-trap combined with gas chromatography-mass spectrometry analysis;
[0029] Figure 9 This is a schematic diagram of the structure of an analytical and detection device for light components in residual oil provided in an embodiment of the present invention;
[0030] Figure 10 This is a schematic diagram of the structure of an electronic device for implementing a method for analyzing and detecting light components in residual oil, as provided in an embodiment of the present invention. Detailed Implementation
[0031] Embodiments of the present invention will now be described in more detail with reference to the accompanying drawings. While some embodiments of the invention are shown in the drawings, it should be understood that the invention can be implemented in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the invention. It should be understood that the accompanying drawings and embodiments are for illustrative purposes only and are not intended to limit the scope of protection of the invention.
[0032] It should be understood that the various steps described in the method embodiments of the present invention may be performed in different orders and / or in parallel. Furthermore, the method embodiments may include additional steps and / or omit the steps shown. The scope of the present invention is not limited in this respect.
[0033] The term "comprising" and its variations as used herein are open-ended inclusions, meaning "including but not limited to". The term "based on" means "at least partially based on". The term "one embodiment" means "at least one embodiment"; the term "another embodiment" means "at least one additional embodiment"; the term "some embodiments" means "at least some embodiments". Definitions of other terms will be given in the description below.
[0034] It should be noted that the concepts of "first" and "second" mentioned in this invention are only used to distinguish different devices, modules or units, and are not used to limit the order of functions performed by these devices, modules or units or their interdependencies.
[0035] It should be noted that the terms "a" and "a plurality of" used in this invention are illustrative rather than restrictive. Those skilled in the art should understand that, unless otherwise expressly indicated in the context, they should be understood as "one or more".
[0036] The names of the messages or information exchanged between the multiple devices in the embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of these messages or information.
[0037] Figure 1This is a schematic flowchart illustrating a method for analyzing and detecting light components in residual oil according to an embodiment of the present invention. This embodiment is applicable to situations requiring rapid and accurate qualitative analysis of light components in residual oil, particularly in the field of petroleum composition analysis, where light components from different sources and processing stages of residual oil are analyzed to optimize process parameters such as delayed coking and residue hydrotreating, thereby improving light oil yield and product quality. This method for analyzing and detecting light components in residual oil can be executed by an analytical device for light components in residual oil. This device can be implemented through software and / or hardware and is generally integrated into any electronic device with network communication capabilities, such as a mobile terminal, PC, or server.
[0038] like Figure 1 As shown, the analytical detection method for light components in residual oil according to embodiments of the present invention may include the following process:
[0039] S110. The sample of residual oil to be tested in the purge trap sampler is purged, and the light components purged from the sample of residual oil to be tested are collected by the trap.
[0040] From a compositional perspective, residual oil is an extremely complex mixture, mainly composed of high-molecular-weight hydrocarbons, sulfur-containing compounds, nitrogen-containing compounds, oxygen-containing compounds, and metallic impurities. The presence of some light components is not negligible. These light components are typically hydrocarbons with relatively small molecular weights and low boiling points, such as C5-C12 alkanes, alkenes, and small amounts of aromatic hydrocarbons. Although they constitute a small proportion of the overall composition of residual oil, they are highly reactive and have a significant impact on its overall properties.
[0041] The purge-trap sampler can be used for sample pretreatment of residual oil samples. Its core function is to effectively extract and enrich volatile components from the sample. It utilizes the purging action of gas to remove light components from the complex matrix. The advantages of using a purge-trap sampler are that it can operate under mild conditions, reducing the impact on the chemical properties of light components, and avoiding impurities that may be introduced by traditional extraction methods, thus providing a pure sample for subsequent analysis.
[0042] A trap can be attached after a purge-and-trap sampler, and its interior is filled with a specific adsorbent (such as activated carbon, Tenax, etc.). The trap is used to capture light components purged from the analyte oil sample. Utilizing the strong adsorption capacity of the adsorbent within the trap, the light components purged from the sample are retained within the trap, achieving efficient enrichment of these components. By employing the highly selective adsorption characteristics of the trap, even trace amounts of light components are ensured to be included, significantly improving the sensitivity of subsequent analyses.
[0043] As an optional but not limited implementation, the residual oil sample to be tested is a residual oil with a volatile odor and containing some light components.
[0044] The volatile odor of residual oil is due to the presence of these light components. Because of their weak intermolecular forces, these light components have high vapor pressures and easily evaporate from the liquid residual oil into the air at room temperature and pressure. When these volatile light components enter the nasal cavity, they stimulate the olfactory nerves, allowing the unique odor of the residual oil to be perceived. This volatile odor not only adversely affects the production environment but may also pose a potential health threat. Furthermore, the volatilization of light components can alter the physical and chemical properties of the residual oil, thus affecting its performance in subsequent processing. For example, when used in the production of road asphalt blending components, excessive volatilization of light components can cause changes in indicators such as penetration and softening point of the asphalt, affecting its quality and performance.
[0045] As an optional but not limited implementation, purging the residual oil sample to be tested in the purge trap sampler includes the following steps:
[0046] After placing 30-50 mg of the residual oil sample to be tested into the purge trap sampler, inert gas at a preset flow rate and volume is introduced into the purge trap sampler for purging. During the purging process, the light components included in the residual oil sample corresponding to the purge trap sampler, due to their high volatility, will escape from the residual oil sample with the inert gas and then enter the trap, so that the adsorbent in the trap can quickly adsorb these light components, thus completing the capture of the light components.
[0047] By employing the aforementioned alternative scheme, the separation of light components from the complex matrix of residual oil is effectively achieved, avoiding the loss and contamination of light components that may occur in traditional separation methods. Simultaneously, the enrichment effect of the trap increases the concentration of light components, providing sufficient sample volume for subsequent analysis and significantly improving analytical sensitivity, enabling accurate detection even of light components present in extremely low concentrations.
[0048] As another optional but not limiting implementation, purging the residual oil sample to be tested in the purge trap sampler includes the following steps:
[0049] According to the preset purging operation, the residual oil sample to be tested in the purging trap sampler is purged. The preset purging operation is configured as follows: under the purging conditions of preset purging preheating temperature and preset transmission line temperature, the residual oil sample to be tested is purged at a preset purging flow rate for a preset purging time. The purging preheating temperature is 40-60℃, the purging time is 2min, the purging transmission line temperature is 190℃, and the purging flow rate is 40mL / min.
[0050] The preset purge preheating temperature refers to the specific temperature that the purge trap injector must reach before purging the residual oil sample. In this scheme, it is set at 40-60℃. This temperature has a critical impact on the residual oil sample. If the temperature is too low, the volatilization rate of light components is slow, making it difficult to effectively separate them from the complex residual oil matrix, resulting in low purge efficiency. If the temperature is too high, it may cause some light components to undergo chemical reactions, changing their original chemical structure and properties, affecting the accuracy of subsequent analysis. A suitable purge preheating temperature can provide favorable conditions for the volatilization of light components, allowing them to escape from the residual oil in a mild environment and ensuring the integrity of the light components.
[0051] The preset transfer line temperature can be the temperature that the transfer line connecting the purge-and-trap injector to the subsequent analytical instrument (such as a gas chromatography-mass spectrometry system) needs to maintain; here, it is set to 190°C. Stable control of the transfer line temperature is crucial to ensure that the purged light components remain gaseous during transport and do not condense on the inner wall of the transfer line due to excessively low temperatures, thus preventing loss of light components and contamination of the transfer line. A suitable transfer line temperature also helps improve the transfer efficiency of light components, allowing them to enter the analytical instrument quickly and stably, ensuring the timeliness and accuracy of the analysis.
[0052] The preset purge flow rate refers to the flow rate of the inert gas (such as nitrogen or helium) introduced into the purge trap sampler during the purge process; in this scheme, it is 40 mL / min. The purge flow rate directly affects the purge effect. If the flow rate is too low, it will not generate sufficient driving force to carry the light components out of the residual oil, resulting in incomplete purge of the light components. If the flow rate is too high, although it can accelerate the purge speed of the light components, it may generate turbulence, causing uneven adsorption of the light components in the trap, and may even carry some unadsorbed light components directly out of the trap, reducing the trapping efficiency. A reasonable purge flow rate can ensure that the light components are fully purged out while ensuring their effective adsorption and enrichment in the trap.
[0053] The preset purging time can be the duration of the purging operation on the residual oil sample to be tested, which is 2 minutes in this case. If the purging time is too short, the light components will not be completely volatilized from the residual oil and purged out, resulting in incomplete analytical results; if the purging time is too long, it will not only waste time and resources, but may also introduce more external interference, affecting the accuracy of the analysis. An appropriate purging time can ensure that as many light components as possible are separated from the residual oil, while avoiding the negative effects of over-purging.
[0054] Based on the experimental requirements and the characteristics of the residual oil sample to be tested, the preset purge preheating temperature, preset transfer line temperature, preset purge flow rate, and preset purge time were set in the control system of the purge trap sampler. The residual oil sample to be tested was placed in the purge trap sampler, and the preset purge operation was initiated. The purge trap sampler began to heat up. When the preset purge preheating temperature of 40-60℃ was reached, inert gas was introduced into the purge trap sampler at a purge flow rate of 40 mL / min to purge the residual oil sample. During the purge process, the transfer line was maintained at the preset temperature of 190℃ to ensure smooth transport of the purged light components. After 2 minutes of continuous purge, the purge operation of the residual oil sample to be tested was completed.
[0055] By precisely controlling these parameters, efficient purging of light components in the residual oil sample was achieved. A suitable preheating temperature for purging allowed the light components to fully volatilize from the residual oil without undergoing chemical changes; a stable transfer line temperature ensured the integrity and stability of the light components during transport; and a reasonable combination of purging flow rate and purging time ensured both complete purging of the light components and effective capture in the trap, improving the separation efficiency and enrichment of the light components. This laid a solid foundation for subsequent capture of light components using the trap and accurate analysis using gas chromatography-mass spectrometry, significantly enhancing the accuracy and reliability of light component analysis in residual oil.
[0056] As an optional but not limited implementation, purging the residual oil sample to be tested in the purge trap sampler includes the following steps:
[0057] When using the purge trap sampler for purging, a preset inert gas is continuously introduced into the purge trap sampler, and the residual oil sample to be tested in the purge trap sampler is purged by the preset inert gas. The preset inert gas is nitrogen.
[0058] The preset inert gas refers to a chemically stable gas that is pre-selected for purging. In this technical solution, the preset inert gas is nitrogen. Due to its extremely stable chemical properties, nitrogen hardly reacts with other substances at room temperature and pressure. This stability ensures that it will not chemically react with the light components in the residual oil sample during purging, and will not change the chemical structure and properties of the light components. This guarantees the integrity of the light components during the purging process and lays the foundation for subsequent accurate analysis of the composition and properties of the light components.
[0059] During the purging process using a purge-and-trap sampler, a pre-set inert gas continuously flows into the sampler. This continuous airflow creates stable purging power, constantly carrying light components from the complex matrix of the residual oil sample. If the gas flow is discontinuous, the escape of light components during the purging process may be unstable, and some light components may not be purged out in time, affecting the separation efficiency of light components and the accuracy of subsequent analysis.
[0060] Before performing the purging operation, check that all components of the purge-and-trap sampler are properly connected to ensure the equipment is in good operating condition. Place the sample tray of the purge-and-trap sampler to be tested in the sample tray and seal it. After setting the inert gas introduction parameters, such as flow rate and pressure, start the preset purging operation, allowing the preset inert gas (such as nitrogen) to be continuously introduced into the purge-and-trap sampler at the set flow rate. As the nitrogen continues to flow in, an airflow is formed in the sample tray of the purge-and-trap sampler, making full contact with the sample. Because the light components in the sample are volatile, they are gradually separated from the sample by the nitrogen airflow and enter the subsequent trapping stage along with the nitrogen.
[0061] By continuously purging the residual oil sample with a pre-set inert gas, efficient separation of light components from the complex matrix of the residual oil was achieved. The chemical stability of nitrogen ensured that the light components did not undergo chemical reactions during the separation process, maintaining their original chemical composition and properties, thus ensuring the reliability of subsequent analysis results for the light components. The continuously introduced nitrogen formed a stable purging force, which could comprehensively and thoroughly purge the light components from the residual oil, improving the separation efficiency and enrichment degree of the light components. This not only provided sufficient sample quantity for the effective capture of light components by the subsequent trap, but also created favorable conditions for the accurate detection and qualitative analysis of light components in the residual oil by analytical instruments such as gas chromatography-mass spectrometry, greatly improving the accuracy and reliability of the entire analytical process.
[0062] S120. Desorb the light components from the residual oil sample to be tested, which are captured by the trap, and introduce them into a gas chromatography-mass spectrometry instrument.
[0063] Desorption is the process of releasing light components from a sample of residual oil that has been adsorbed into a trap. By changing conditions such as temperature and pressure, the interaction between the light components and the adsorbent in the trap is weakened, causing them to detach from the adsorbent surface and enter the gas chromatography-mass spectrometry (GC-MS) instrument for analysis. The desorption process directly affects the integrity and accuracy of the light components entering the analytical instrument.
[0064] Gas chromatography-mass spectrometry (GC-MS) is a powerful analytical instrument that combines the high separation efficiency of GC with the precise qualitative capabilities of mass spectrometry. The GC portion utilizes the differences in partition coefficients between the stationary and mobile phases to separate the light component mixture in the desorbed analyte oil sample into individual components. The mass spectrometry portion ionizes the separated components and determines the molecular weight and structural information of the compounds based on their mass-to-charge ratios. By comparing with a standard spectral library, accurate identification of various compounds within the light components is achieved.
[0065] As an optional but not limited implementation, the light components in the residual oil sample to be tested, captured in the trap, are desorbed and introduced into a gas chromatography-mass spectrometry (GC-MS) instrument. This includes: performing desorption operations such as heating or reducing pressure on the trap containing the light components, so that the light components in the residual oil sample to be tested are desorbed from the adsorbent in the trap. The desorbed light components in the residual oil sample to be tested are then directly introduced into the GC-MS instrument via a transfer line, ready for analysis and detection.
[0066] By adopting the above-mentioned optional schemes, the loss and contamination risk of light components during the transfer process are reduced, ensuring the integrity and purity of light components when they enter the analytical instrument. The direct injection method simplifies the operation process, improves analytical efficiency, and avoids interference from external factors on light components, thus laying the foundation for accurate qualitative analysis.
[0067] As an optional but not limited implementation, the light components in the residual oil sample to be tested, captured by the trap, are desorbed and introduced into a gas chromatography-mass spectrometry (GC-MS) instrument, including the following steps:
[0068] A preset desorption operation is performed on the light components in the residue oil sample collected by the trap. The light components in the residue oil sample collected by the trap are desorbed into the gas chromatography-mass spectrometry (GC-MS) instrument. The preset desorption operation is configured as follows: the light components in the residue oil are desorbed into the GC-MS instrument at a preset desorption temperature and within a preset desorption time. The preset desorption temperature is 210℃ and the preset desorption time is 1 min.
[0069] The preset desorption temperature refers to the temperature set beforehand during the desorption operation. In this scheme, it can be set to 210℃. This temperature plays a decisive role in the desorption effect of light components. If the temperature is too low, the interaction force between the light components and the adsorbent in the trap cannot be effectively weakened, resulting in incomplete desorption of the light components and insufficient content of light components entering the gas chromatography-mass spectrometry (GC-MS) instrument, affecting the sensitivity and accuracy of the analysis. On the other hand, if the temperature is too high, it may cause thermal decomposition or other chemical reactions of the light components, changing their original chemical structure, which will also interfere with the subsequent analytical results. The preset desorption temperature can be obtained through experimental verification, ensuring sufficient desorption of light components while minimizing changes in their chemical properties.
[0070] The preset desorption time can be the duration of the desorption process of light components in the residual oil sample to be tested; here it is set to 1 minute. If the desorption time is too short, the light components cannot be completely removed from the adsorbent, resulting in some light components remaining and reducing the integrity of the analysis; if the desorption time is too long, it may introduce more external interference, and will also increase the analysis time cost and reduce work efficiency. The preset desorption time can ensure that the light components are fully desorbed within an appropriate time, balancing the desorption effect and the analysis efficiency.
[0071] The trap, as an enrichment device for light components, is filled with an adsorbent that strongly adsorbs light components. During the initial purging process, it efficiently captures light components purged from the residual oil sample, achieving concentration. In the desorption stage, the trap is the site of light component desorption, and its performance and the characteristics of the internal adsorbent directly affect the desorption efficiency.
[0072] After capturing the light components in the residual oil sample, connect the trap to the gas chromatography-mass spectrometry (GC-MS) instrument using a dedicated transfer line, ensuring a tight and leak-free connection. Set the preset desorption temperature to 210℃ and the preset desorption time to 1 min. Initiate the preset desorption operation; the trap begins to heat up. Once the preset desorption temperature of 210℃ is reached, maintain this temperature for 1 min. During this 1 min, due to the increased temperature, the intermolecular forces between the light components and the adsorbent weaken, and the light components gradually desorb from the adsorbent surface. The desorbed light components, carried by the carrier gas (usually helium), are rapidly transported through the transfer line into the GC-MS instrument, ready for subsequent analysis and detection.
[0073] By controlling the preset desorption temperature and time, efficient desorption and accurate injection of light components in the trap are achieved. The desorption temperature ensures that the light components are fully removed from the adsorbent, guaranteeing a sufficient concentration of light components entering the gas chromatography-mass spectrometry (GC-MS) instrument and improving analytical sensitivity. The preset desorption time ensures complete desorption of light components while avoiding interference and efficiency reduction caused by excessively long desorption times. Through this desorption operation, the light components enter the GC-MS instrument in a complete and pure state, providing excellent sample conditions for efficient separation and accurate qualitative analysis of light components. This significantly improves the accuracy and reliability of light component analysis in residual oils and contributes to a deeper understanding of the chemical composition and properties of residual oils.
[0074] S130. Gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample.
[0075] The light components entering the gas chromatography-mass spectrometry (GC-MS) system are first separated in the gas chromatography column. Based on the different partition coefficients of each component between the stationary and mobile phases, each component is separated individually. The separated components then sequentially enter the mass spectrometer, where they are ionized in the ion source. Finally, they are separated and detected in the mass analyzer according to their mass-to-charge ratio, resulting in mass spectra for each component. By comparing these spectra with data from a standard spectral library, the structures and types of various compounds within the light components are determined.
[0076] Leveraging the powerful capabilities of gas chromatography-mass spectrometry (GC-MS), comprehensive and accurate qualitative analysis of light components in residual oil samples can be performed. This analytical method not only identifies the compounds present in the light components but also provides structural information about these compounds, offering detailed data support for a deeper understanding of the chemical composition of residual oils. This contributes to scientific decision-making in various fields such as petrochemicals and environmental protection.
[0077] As an optional but not limited approach, gas chromatography-mass spectrometry (GC-MS) is used to perform qualitative analysis and detection of light components in the desorbed residual oil sample, including the following steps:
[0078] According to the preset gas chromatography conditions, gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample;
[0079] The preset gas chromatography conditions are configured as follows: the gas chromatography-mass spectrometry (GC-MS) instrument uses a 30m×0.25mm×0.25μm column in constant flow mode with a flow rate of 1.0mL / min; the GC-MS instrument uses a 280℃ injection temperature and a split injection mode with a split ratio of N:1, where N is 50-100; the column temperature is configured as follows: the initial temperature of the column is set to 35℃ and held for 5min; the column temperature is then increased to 80℃ at a rate of 2℃ / min, held for 2min, increased to 150℃ at a rate of 5℃ / min, and then increased to 300℃ at a rate of 10℃ / min.
[0080] Gas chromatography-mass spectrometry (GC-MS) integrates the powerful separation capabilities of GC with the precise qualitative and quantitative capabilities of mass spectrometry. GC separates components in complex mixtures based on the differences in partition coefficients between the stationary and mobile phases; mass spectrometry, on the other hand, ionizes the separated components and determines the molecular weight, structure, and other information of the compounds based on the mass-to-charge ratio of the ions, thus enabling comprehensive analysis of all components in complex samples. It is a core instrument in the analysis of light components in residual oils, providing the foundation for obtaining accurate qualitative results.
[0081] The chromatographic column used in this protocol is a 30m × 0.25mm × 0.25μm column. The 30m column length provides a larger separation space, increasing the number of partitions of each light component between the stationary and mobile phases, thereby improving separation efficiency and enabling effective separation of light components with similar properties. The 0.25mm inner diameter determines the degree of sample diffusion and mass transfer resistance within the column; a smaller inner diameter helps reduce longitudinal diffusion, improves column efficiency, obtains sharper chromatographic peaks, and enhances separation performance. The 0.25μm stationary phase film thickness affects the interaction between the components and the stationary phase; an appropriate film thickness ensures suitable retention times and selectivity for each light component within the column, guaranteeing accurate separation.
[0082] The constant flow mode was set to 1.0 mL / min. In constant flow mode, the carrier gas flow rate remains stable, which ensures a stable migration rate of the sample within the column, facilitating the establishment of a stable partition equilibrium between the stationary and mobile phases for the light components. The stable flow rate also guarantees good reproducibility of peak retention times, facilitating qualitative comparison with standard spectra and contributing to improved accuracy and precision of the analytical results.
[0083] The injection port temperature is set to 280℃, which is crucial for sample vaporization and injection efficiency. If the temperature is too low, the light components of the residual oil will not completely vaporize, leading to inaccurate injection volume, peak tailing, and affecting separation and qualitative analysis. If the temperature is too high, the light components may undergo thermal decomposition or chemical reactions, altering their chemical structure and interfering with the analytical results. The injection port temperature ensures that the light components are rapidly and completely vaporized, smoothly entering the chromatographic column in gaseous form for separation.
[0084] A split ratio of N:1 is used in the split injection mode, where N is 50-100. Split injection mode is suitable for high sample concentrations. By splitting, the amount of sample entering the column is reduced, avoiding column overload and ensuring good separation. A suitable split ratio ensures that the amount of sample entering the column is within the instrument's linear response range, improving analytical accuracy. When analyzing light components in residual oils, where the content of light components may be high, a split ratio of 50-100 can effectively control the injection volume and ensure analytical reliability.
[0085] Regarding the column temperature settings, the initial column temperature was set to 35℃ and held for 5 minutes. This lower initial temperature allows low-boiling-point light components to accumulate sufficiently at the column tip, forming sharp peaks and improving resolution. Then, the temperature was increased to 80℃ at a rate of 2℃ / min and held for 2 minutes. This heating rate and isothermal process helps separate light components with similar boiling points, further optimizing the separation effect. Next, the temperature was increased to 150℃ at a rate of 5℃ / min, and then further increased to 300℃ at a rate of 10℃ / min. This gradual increase in temperature allows high-boiling-point light components to elute sequentially from the column, achieving comprehensive separation of light components with different boiling point ranges.
[0086] The light components, desorbed from the trap, are introduced into the injection port of the gas chromatography-mass spectrometry (GC-MS) instrument via a transfer line. In the instrument's control software, parameters are set according to preset GC conditions, including selecting a 30m × 0.25mm × 0.25μm column, setting a constant flow mode of 1.0mL / min, an injection port temperature of 280℃, a split injection mode with a split ratio of N:1, and setting the column temperature change program. After setting, the instrument analysis program is started. The light component sample rapidly vaporizes at the injection port and enters the chromatographic column under the carry gas. In the column, each light component gradually separates under different temperature conditions based on the difference in their partition coefficients between the stationary and mobile phases. The separated light components sequentially enter the mass spectrometer, are ionized in the ion source, and then separated and detected in the mass analyzer according to their mass-to-charge ratio, ultimately obtaining the mass spectrum of each light component. By comparing the obtained mass spectra with data in a standard spectral library, the compound types and structures of the light components in the residual oil are determined.
[0087] By operating under preset gas chromatography conditions, efficient separation and accurate qualitative analysis of light components in residual oil are achieved. Appropriate column specifications and constant flow mode ensure good separation and stable retention times for each light component within the column. Inlet temperature and split ratio ensure effective sample injection and normal column operation. Precise column temperature control programs enable comprehensive and precise separation of light components within different boiling point ranges. The synergistic effect of these conditions allows gas chromatography-mass spectrometry (GC-MS) to accurately detect and identify light components in residual oil, providing detailed and reliable data support for a deeper understanding of its chemical composition. This contributes to scientific decision-making in fields such as petrochemicals and environmental protection, including optimizing residual oil processing techniques and assessing its potential environmental impact.
[0088] As an optional but not limited implementation scheme, the chromatographic column corresponding to the gas chromatography-mass spectrometry system in this scheme is an HP-5MS (30m×0.25mm×0.25μm) flexible quartz tube capillary column.
[0089] As an optional but not limited implementation, the residual oil sample to be tested is at least one of the following types of residual oil: heavy oil, slurry oil, fuel oil, coking wax oil, and waste lubricating oil.
[0090] Heavy oil is a special type of petroleum resource whose formation is closely related to geological conditions. It typically develops over a long geological evolution process, where crude oil undergoes various processes such as biodegradation, water washing, and oxidation, leading to the gradual loss of light components and the relative enrichment of heavy components, resulting in high viscosity and density. Heavy oil contains a large amount of gum and asphaltenes, as well as some light components, which significantly impact its extraction, transportation, and processing. For example, during extraction, the presence of light components affects its fluidity, requiring specialized techniques such as steam injection and hot water injection; during transportation, the volatilization of light components can lead to scaling and corrosion in pipelines. Therefore, analyzing the light components in heavy oil helps optimize extraction and transportation processes, improving extraction efficiency and transportation safety.
[0091] Oil slurry is a byproduct of petroleum refining processes, such as catalytic cracking units producing light oil products. It consists of unconverted heavy hydrocarbons, fine catalyst powder, and small amounts of light components. Although the content of light components in oil slurry is relatively small, it affects its properties and subsequent utilization. In industrial production, oil slurry is often used to produce road asphalt blending components, rubber softeners, etc. If the content of light components in the oil slurry is too high, it will affect the quality and stability of the products. Therefore, analyzing the light components in oil slurry is crucial for the rational utilization of oil slurry resources and the improvement of product quality.
[0092] Fuel oil is an important energy source widely used in industry and shipbuilding. It is primarily derived from crude oil through distillation, cracking, and blending processes. Fuel oil has a complex composition, containing not only a large amount of hydrocarbons but also impurities such as sulfur, nitrogen, and oxygen, as well as some light components. During the storage and transportation of fuel oil, the volatilization of these light components not only wastes energy but can also pose safety hazards, such as forming flammable mixtures that could lead to explosions. Furthermore, during combustion, the content and properties of these light components affect the combustion efficiency and pollutant emissions of fuel oil. Therefore, analyzing the light components in fuel oil helps ensure its safe storage and transportation, optimize the combustion process, and reduce environmental pollution.
[0093] Coking wax oil is a product obtained from crude oil through a delayed coking process. Delayed coking is an important process for converting heavy oil into light oil and coke, during which coking wax oil is produced. Coking wax oil contains a significant amount of aromatics and heterocyclic compounds, as well as a certain amount of light components. Coking wax oil can be used as a feedstock for further processing, such as in the production of diesel fuel and lubricating oil base oils. However, the light components can affect subsequent processing techniques and product quality. For example, during hydrorefining, the presence of light components may lead to changes in reaction conditions, affecting the hydrorefining effect. Therefore, analyzing the light components in coking wax oil is of great significance for optimizing subsequent processing techniques and improving product quality.
[0094] Waste lubricating oil refers to the used oil products generated during the operation of various mechanical equipment. Due to the introduction of impurities and additives during use, as well as oxidation, its composition becomes complex and diverse. Waste lubricating oil not only contains residual components of base oil but also a large amount of metal shavings, dust, moisture, and decomposition products of additives, as well as some light components. Indiscriminate discharge of waste lubricating oil can cause serious pollution to soil and water bodies. Analyzing the light components in waste lubricating oil helps to understand its composition and properties, providing a basis for developing reasonable recycling and treatment processes, realizing the resource utilization of waste lubricating oil, and reducing environmental pollution.
[0095] Optionally, taking heavy oil as an example, 30-50 mg of heavy oil sample is weighed into a 40 mL purge-and-trap injector for pretreatment using a purge-and-trap instrument. The sample is then purged for 2 min at a nitrogen flow rate of 40 mL / min under preheating conditions of 40-60℃, followed by desorption into a gas chromatography-mass spectrometry (GC-MS) system for compositional analysis within 1 min. The chromatographic column used in the GC-MS is an HP-5MS (30 m × 0.25 mm × 0.25 μm) flexible quartz tube capillary column; the injection port temperature is 280℃; the column oven temperature program is: 35℃ held for 5 min, increased to 80℃ at 2℃ / min, held for 2 min, increased to 150℃ at 5℃ / min, and then increased to 300℃ at 10℃; the mass spectrometer uses an EI ionization source; the scanning mode is full scan; the scan range is m / z 35-500; and the scan frequency is 0.3 s. The light components in the residual oil were analyzed using purge-and-trap combined with gas chromatography-mass spectrometry to determine their chemical composition. The analytical results are as follows: Figure 2 As shown, Figure 2 The image shows the total ion chromatogram of the light components in the heavy oil sample, and the compositional characteristics of the light components in the heavy oil were determined based on m / z 85. Through mass spectrometry fragment comparison, the main chromatographic peaks were identified as hydrocarbon compounds.
[0096] Optionally, taking heavy oil as the sample to be tested, this embodiment provides a comparative experimental analysis of light components in heavy oil. The only difference is the purging heating temperature; in the comparative experiment, the purging heating temperature is 25℃ instead of 40-60℃. The analytical results are as follows: Figure 3 As shown, based on the composition of light components in heavy oil, it was determined that light components were not effectively detected under the purging conditions.
[0097] Optionally, taking heavy oil as the sample to be tested, this embodiment provides a comparative experimental analysis of light components in heavy oil. The only difference is the purging time; in the comparative experiment, the purging time is 6 minutes instead of 2 minutes. The analytical results are as follows: Figure 4 As shown, based on the composition of the light components in the heavy oil, it is determined that the heavy components carried out under this purging condition may cause contamination of the chromatographic column and instruments.
[0098] Optionally, this embodiment uses the same process as for the heavy oil in the previous example to analyze the light component compounds in the oil slurry. Figure 5 The GC-MS total ion chromatogram of the light components in this oil slurry sample shows that the composition of the light components in the oil slurry is significantly different from that of the heavy oil in the previous example. The oil slurry contains abundant benzene compounds, mainly including benzene, toluene, xylene, and trimethylbenzene compounds. This example illustrates that the analytical method of the present invention has good applicability to different types of samples.
[0099] Optionally, this embodiment uses the same process as for heavy oil in the aforementioned examples to analyze light component compounds in fuel oil. Figure 6 This is the GC-MS total ion chromatogram of the light components in the fuel oil sample. The fuel oil contains C8-C15 hydrocarbons, and the abundance of high-carbon-number compounds is higher compared to other residual oil samples. In addition, C1-C4 benzene series compounds and naphthalene compounds were detected in the fuel oil.
[0100] Optionally, this embodiment uses the same process as the heavy oil in the previous example to analyze the light component compounds in the coking wax oil. Figure 7 This is the GC-MS total ion chromatogram of the light components in the coking wax oil sample. The hydrocarbons in the coking wax oil have a carbon number distribution of C8-C15, with lower carbon number compounds being less abundant. In addition, benzene series compounds and polycyclic aromatic hydrocarbons were also detected in the coking wax oil.
[0101] Optionally, this embodiment uses the same process as the heavy oil in the previous example to analyze the light component compounds in the waste lubricating oil. Figure 8 This is the GC-MS total ion chromatogram of the light components in the waste lubricating oil sample. The main detected compounds in the waste lubricating oil are C1-C3 benzene series and C8-C16 alkane compounds.
[0102] This invention utilizes a purge-and-trap pretreatment device to separate and trap light components in residual oil, followed by gas chromatography-mass spectrometry (GC-MS) to analyze the molecular composition of these light components. This effectively solves the problem of existing technologies being unable to directly analyze the molecular composition of light components in residual oil. Furthermore, the analytical method for analyzing the composition of light components in residual oil provided by this invention is applicable to the analysis of heavy oil, fuel oil, waste lubricating oil, slurry oil, and coking wax oil samples. It enables simple and efficient analysis of the molecular composition of light components in residual oil, reduces the loss of light components during pretreatment, and avoids contamination of the chromatographic column and GC-MS instrument during the analysis process.
[0103] The technical solution of this invention addresses the challenge of separating highly volatile light components from a complex matrix in residual oil. Traditional methods struggle to effectively separate these components. By using a purge-and-trap sampler to purge the residual oil sample, the flow of gas can separate these components from the complex matrix. Furthermore, the use of a trap ensures efficient capture of the purged light components, even those present in extremely low concentrations. The captured light components are then desorbed and directly introduced into a gas chromatography-mass spectrometry (GC-MS) instrument. This reduces loss and contamination of light components during transfer. GC then separates the desorbed mixture of light components based on their partition coefficients between the stationary and mobile phases, allowing each component to sequentially enter the mass spectrometer. This enables accurate identification of various compounds within the light components. Qualitative analysis of the light components in the residual oil provides a deeper understanding of its chemical composition, offering crucial information for its processing and utilization.
[0104] Figure 9 This is a schematic diagram of the structure of an analytical detection device for light components in residual oil provided in an embodiment of the present invention. The present invention is applicable to situations where light components in residual oil are rapidly and accurately analyzed, especially in the field of petroleum composition analysis, to analyze light components in residual oil from different sources and processing stages, thereby optimizing process parameters such as delayed coking and residue hydrotreating, and improving the yield and quality of light oil. The analytical detection device for light components in residual oil can be implemented in the form of software and / or hardware, and is generally integrated into any electronic device with network communication capabilities, such as a mobile terminal, PC, or server.
[0105] like Figure 9 As shown, the analytical and detection device for light components in residual oil according to an embodiment of the present invention may include:
[0106] The purge and trap module 910 is used to purge the residual oil sample to be tested in the purge and trap sampler and to capture the light components purged from the residual oil sample to be tested through the trap.
[0107] The desorption module 920 is used to desorb the light components in the residual oil sample to be tested captured by the trap and introduce them into the gas chromatography-mass spectrometry instrument.
[0108] The analysis and detection module 930 is used to perform qualitative analysis and detection of light components in the desorbed residue oil sample using a gas chromatography-mass spectrometry system.
[0109] Based on the above embodiments, optionally, the residual oil sample to be tested in the purge trap sampler is purged, including:
[0110] According to the preset purging operation, the residual oil sample to be tested in the purging trap sampler is purged. The preset purging operation is configured as follows: under the purging conditions of preset purging preheating temperature and preset transmission line temperature, the residual oil sample to be tested is purged at a preset purging flow rate for a preset purging time. The purging preheating temperature is 40-60℃, the purging time is 2min, the purging transmission line temperature is 190℃, and the purging flow rate is 40mL / min.
[0111] Based on the above embodiments, optionally, the residual oil sample to be tested in the purge trap sampler is purged, including:
[0112] When using the purge trap sampler for purging, a preset inert gas is continuously introduced into the purge trap sampler, and the residual oil sample to be tested in the purge trap sampler is purged by the preset inert gas.
[0113] Optionally, based on the above embodiments, the preset inert gas is nitrogen.
[0114] Based on the above embodiments, optionally, the light components in the residual oil sample to be tested captured by the trap are desorbed and introduced into a gas chromatography-mass spectrometry instrument, including:
[0115] A preset desorption operation is performed on the light components in the residue oil sample to be tested, which is captured in the trap, to desorb the light components into the gas chromatography-mass spectrometry (GC-MS) instrument. The preset desorption operation is configured as follows: the light components in the residue oil are desorbed into the GC-MS instrument at a preset desorption temperature and within a preset desorption time. The preset desorption temperature is 210°C and the preset desorption time is 1 min.
[0116] Based on the above embodiments, optionally, the residual oil sample to be tested is a residual oil with a volatile odor and containing some light components.
[0117] Based on the above embodiments, optionally, the residual oil sample to be tested is at least one of the following types of residual oil: heavy oil, slurry oil, fuel oil, coking wax oil, and waste lubricating oil.
[0118] Based on the above embodiments, optionally, gas chromatography-mass spectrometry (GC-MS) is used to perform qualitative analysis and detection of light components in the desorbed residual oil sample, including:
[0119] According to the preset gas chromatography conditions, gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample;
[0120] The preset gas chromatography conditions are configured as follows: the gas chromatography-mass spectrometry (GC-MS) instrument uses a 30m×0.25mm×0.25μm column in constant flow mode with a flow rate of 1.0mL / min; the GC-MS instrument uses a split injection mode with an injection port temperature of 280℃ and a split ratio of N:1, where N is 50-100; the column temperature is configured as follows: the initial temperature of the column is set to 35℃ and held for 5min; the column temperature is then increased to 80℃ at a rate of 2℃ / min, held for 2min, increased to 150℃ at a rate of 5℃ / min, and then increased to 300℃ at a rate of 10℃ / min.
[0121] The technical solution of this invention addresses the challenge of separating highly volatile light components from a complex matrix in residual oil. Traditional methods struggle to effectively separate these components. By using a purge-and-trap sampler to purge the residual oil sample, the flow of gas can separate these components from the complex matrix. Furthermore, the use of a trap ensures efficient capture of the purged light components, even those present in extremely low concentrations. The captured light components are then desorbed and directly introduced into a gas chromatography-mass spectrometry (GC-MS) instrument. This reduces loss and contamination of light components during transfer. GC then separates the desorbed mixture of light components based on their partition coefficients between the stationary and mobile phases, allowing each component to sequentially enter the mass spectrometer. This enables accurate identification of various compounds within the light components. Qualitative analysis of the light components in the residual oil provides a deeper understanding of its chemical composition, offering crucial information for its processing and utilization.
[0122] The analytical detection device for light components in residual oil provided in this embodiment of the invention can execute the analytical detection method for light components in residual oil provided in any embodiment of the invention, and has the corresponding functional modules and beneficial effects for executing the analytical detection method for light components in residual oil.
[0123] It is worth noting that the various units and modules included in the above-mentioned device are only divided according to functional logic, but are not limited to the above division, as long as the corresponding functions can be realized; in addition, the specific names of each functional unit are only for easy differentiation and are not used to limit the protection scope of the embodiments of the present invention.
[0124] Figure 10 This is a schematic diagram of an electronic device for implementing a method for analyzing and detecting light components in residual oil, as provided in an embodiment of the present invention. The following refers to... Figure 10 It illustrates an electronic device suitable for implementing embodiments of the present invention (e.g., Figure 10 The diagram below shows the structure of the terminal device or server 1000. The terminal device in this embodiment may include, but is not limited to, mobile terminals such as mobile phones, laptops, digital broadcast receivers, PDAs (personal digital assistants), PADs (tablet computers), PMPs (portable multimedia players), and vehicle terminals (e.g., vehicle navigation terminals), as well as fixed terminals such as digital TVs and desktop computers. Figure 10 The electronic device shown is merely an example and should not be construed as limiting the functionality and scope of use of the embodiments of the present invention.
[0125] like Figure 10 As shown, the electronic device 1000 may include a processing unit (e.g., a central processing unit, a graphics processing unit, etc.) 1001, which can perform various appropriate actions and processes according to a program stored in a read-only memory (ROM) 1002 or a program loaded from a storage device 1008 into a random access memory (RAM) 1003. The RAM 1003 also stores various programs and data required for the operation of the electronic device 1000. The processing unit 1001, ROM 1002, and RAM 1003 are interconnected via a bus 1004. An edit / output (I / O) interface 1005 is also connected to the bus 1004.
[0126] Typically, the following devices can be connected to the I / O interface 1005: input devices 1006 including, for example, a touchscreen, touchpad, keyboard, mouse, camera, microphone, accelerometer, gyroscope, etc.; output devices 1007 including, for example, a liquid crystal display (LCD), speaker, vibrator, etc.; storage devices 1008 including, for example, magnetic tape, hard disk, etc.; and communication devices 1009. Communication device 1009 allows electronic device 1000 to communicate wirelessly or wiredly with other devices to exchange data. Although Figure 10 An electronic device 1000 with various devices is shown; however, it should be understood that it is not required to implement or possess all of the devices shown. More or fewer devices may be implemented or possessed alternatively.
[0127] In particular, according to embodiments of the present invention, the processes described above with reference to the flowchart can be implemented as computer software programs. For example, embodiments of the present invention include a computer program product comprising a computer program carried on a non-transitory computer-readable medium, the computer program containing program code for performing the analytical detection method for light components in residual oil shown in the flowchart. In such embodiments, the computer program can be downloaded and installed from a network via a communication device 1009, or installed from a storage device 1008, or installed from a ROM 1002. When the computer program is executed by the processing device 1001, it performs the functions defined in the analytical detection method for light components in residual oil according to embodiments of the present invention.
[0128] The names of the messages or information exchanged between the multiple devices in the embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of these messages or information.
[0129] The electronic device provided in this embodiment of the invention and the method for analyzing and detecting light components in residual oil provided in the above embodiments belong to the same inventive concept. Technical details not described in detail in this embodiment can be found in the above embodiments, and this embodiment has the same beneficial effects as the above embodiments.
[0130] This invention provides a computer storage medium storing a computer program that, when executed by a processor, implements the analytical detection method for light components in residual oil provided in the above embodiments.
[0131] It should be noted that the computer-readable medium described above in this invention can be a computer-readable signal medium, a computer-readable storage medium, or any combination thereof. A computer-readable storage medium can be, for example,—but not limited to—an electrical, magnetic, optical, electromagnetic, infrared, or semiconductor system, apparatus, or device, or any combination thereof. More specific examples of a computer-readable storage medium may include, but are not limited to: an electrical connection having one or more wires, a portable computer disk, a hard disk, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EPROM or flash memory), optical fiber, portable compact disk read-only memory (CD-ROM), optical storage device, magnetic storage device, or any suitable combination thereof. In this invention, a computer-readable storage medium can be any tangible medium containing or storing a program that can be used by or in conjunction with an instruction execution system, apparatus, or device. In this invention, a computer-readable signal medium can include a data signal propagated in baseband or as part of a carrier wave, carrying computer-readable program code. Such propagated data signals can take various forms, including but not limited to electromagnetic signals, optical signals, or any suitable combination thereof. A computer-readable signal medium can be any computer-readable medium other than a computer-readable storage medium, which can send, propagate, or transmit a program for use by or in connection with an instruction execution system, apparatus, or device. The program code contained on the computer-readable medium can be transmitted using any suitable medium, including but not limited to: wires, optical fibers, RF (radio frequency), etc., or any suitable combination thereof.
[0132] In some implementations, clients and servers can communicate using any currently known or future-developed network protocol such as HTTP (Hypertext Transfer Protocol) and can interconnect with digital data communication (e.g., communication networks) of any form or medium. Examples of communication networks include local area networks (“LANs”), wide area networks (“WANs”), the Internet (e.g., the Internet of Things), and peer-to-peer networks (e.g., ad hoc peer-to-peer networks), as well as any currently known or future-developed networks.
[0133] The aforementioned computer-readable medium may be included in the aforementioned electronic device; or it may exist independently and not assembled into the electronic device.
[0134] The aforementioned computer-readable medium carries one or more programs, which, when executed by the electronic device, cause the electronic device to: purge the test residue oil sample in the purge trap and collect the light components purged from the test residue oil sample through the trap; desorb the light components in the test residue oil sample collected by the trap into a gas chromatography-mass spectrometry (GC-MS) instrument; and perform qualitative analysis and detection of the desorbed light components in the test residue oil sample using the GC-MS instrument.
[0135] Computer program code for performing the operations of this invention can be written in one or more programming languages or a combination thereof, including but not limited to object-oriented programming languages such as Java, Smalltalk, and C++, as well as conventional procedural programming languages such as the "C" language or similar programming languages. The program code can be executed entirely on the user's computer, partially on the user's computer, as a standalone software package, partially on the user's computer and partially on a remote computer, or entirely on a remote computer or server. In cases involving remote computers, the remote computer can be connected to the user's computer via any type of network—including a local area network (LAN) or a wide area network (WAN)—or can be connected to an external computer (e.g., via the Internet using an Internet service provider).
[0136] The flowcharts and block diagrams in the accompanying drawings illustrate the architecture, functionality, and operation of possible implementations of systems, methods, and computer program products according to various embodiments of the present invention. In this regard, each block in a flowchart or block diagram may represent a module, segment, or portion of code containing one or more executable instructions for implementing a specified logical function. It should also be noted that in some alternative implementations, the functions indicated in the blocks may occur in a different order than those indicated in the drawings. For example, two consecutively indicated blocks may actually be executed substantially in parallel, and they may sometimes be executed in reverse order, depending on the functions involved. It should also be noted that each block in the block diagrams and / or flowcharts, and combinations of blocks in the block diagrams and / or flowcharts, can be implemented using a dedicated hardware-based system that performs the specified function or operation, or using a combination of dedicated hardware and computer instructions.
[0137] The units described in the embodiments of the present invention can be implemented in software or in hardware. The name of a unit does not necessarily limit the unit itself; for example, the first acquisition unit can also be described as "a unit that acquires at least two Internet Protocol addresses".
[0138] The functions described above in this document can be performed, at least in part, by one or more hardware logic components. For example, exemplary types of hardware logic components that can be used, without limitation, include: Field Programmable Gate Arrays (FPGAs), Application-Specific Integrated Circuits (ASICs), Application Standard Products (ASSPs), System-on-Chip (SoCs), Complex Programmable Logic Devices (CPLDs), and so on.
[0139] In the context of this invention, a machine-readable medium can be a tangible medium that may contain or store a program for use by or in conjunction with an instruction execution system, apparatus, or device. A machine-readable medium can be a machine-readable signal medium or a machine-readable storage medium. Machine-readable media can include, but are not limited to, electronic, magnetic, optical, electromagnetic, infrared, or semiconductor systems, apparatus, or devices, or any suitable combination of the foregoing. More specific examples of machine-readable storage media include electrical connections based on one or more wires, portable computer disks, hard disks, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EPROM or flash memory), optical fibers, portable compact disk read-only memory (CD-ROM), optical storage devices, magnetic storage devices, or any suitable combination of the foregoing.
[0140] The above description is merely a preferred embodiment of the present invention and an explanation of the technical principles employed. Those skilled in the art should understand that the scope of disclosure in this invention is not limited to technical solutions formed by specific combinations of the above-described technical features, but should also cover other technical solutions formed by arbitrary combinations of the above-described technical features or their equivalents without departing from the above-described concept. For example, technical solutions formed by substituting the above features with (but not limited to) technical features with similar functions disclosed in this invention.
[0141] Furthermore, while the operations are described in a specific order, this should not be construed as requiring these operations to be performed in the specific order shown or in sequential order. In certain circumstances, multitasking and parallel processing may be advantageous. Similarly, while several specific implementation details are included in the above discussion, these should not be construed as limiting the scope of the invention. Certain features described in the context of individual embodiments may also be implemented in combination in a single embodiment. Conversely, various features described in the context of a single embodiment may also be implemented individually or in any suitable sub-combination in multiple embodiments.
[0142] Although the subject matter has been described using language specific to structural features and / or methodological logic, it should be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or actions described above. Rather, the specific features and actions described above are merely illustrative examples of implementing the claims.
Claims
1. A method for analyzing and detecting light components in residual oil, characterized in that, The method includes: The residual oil sample to be tested is purged in the purge trap sampler, and the light components purged from the residual oil sample are collected by the trap. The light components in the residual oil sample to be tested, captured by the trap, are desorbed and introduced into a gas chromatography-mass spectrometry instrument. Gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample.
2. The method according to claim 1, characterized in that, The residual oil sample to be tested in the purge trap sampler is purged, including: According to the preset purging operation, the residual oil sample to be tested in the purging trap sampler is purged. The preset purging operation is configured as follows: under the purging conditions of preset purging preheating temperature and preset transmission line temperature, the residual oil sample to be tested is purged at a preset purging flow rate for a preset purging time. The purging preheating temperature is 40-60℃, the purging time is 2min, the purging transmission line temperature is 190℃, and the purging flow rate is 40mL / min.
3. The method according to claim 1 or 2, characterized in that, The residual oil sample to be tested in the purge trap sampler is purged, including: When using the purge trap sampler for purging, a preset inert gas is continuously introduced into the purge trap sampler, and the residual oil sample to be tested in the purge trap sampler is purged by the preset inert gas.
4. The method according to claim 1, characterized in that, The light components in the residual oil sample to be tested, captured by the trap, are desorbed and introduced into a gas chromatography-mass spectrometry system, including: A preset desorption operation is performed on the light components in the residue oil sample to be tested, which is captured in the trap, to desorb the light components into the gas chromatography-mass spectrometry (GC-MS) instrument. The preset desorption operation is configured as follows: the light components in the residue oil are desorbed into the GC-MS instrument at a preset desorption temperature and within a preset desorption time. The preset desorption temperature is 210°C and the preset desorption time is 1 min.
5. The method according to claim 1, characterized in that, The residual oil sample to be tested is a residual oil with a volatile odor and containing some light components.
6. The method according to claim 5, characterized in that, The residual oil sample to be tested is at least one of the following types of residual oil: heavy oil, slurry oil, fuel oil, coking wax oil, and waste lubricating oil.
7. The method according to claim 1, characterized in that, The light components in the desorbed residual oil sample were qualitatively analyzed using gas chromatography-mass spectrometry, including: According to the preset gas chromatography conditions, gas chromatography-mass spectrometry was used to perform qualitative analysis and detection of light components in the desorbed residual oil sample; The preset gas chromatography conditions are configured as follows: the gas chromatography-mass spectrometry (GC-MS) instrument uses a 30m×0.25mm×0.25μm column in constant flow mode with a flow rate of 1.0mL / min; the GC-MS instrument uses a split injection mode with an injection port temperature of 280℃ and a split ratio of N:1, where N is 50-100; the column temperature is configured as follows: the initial temperature of the column is set to 35℃ and held for 5min; the column temperature is then increased to 80℃ at a rate of 2℃ / min, held for 2min, increased to 150℃ at a rate of 5℃ / min, and then increased to 300℃ at a rate of 10℃ / min.
8. An analytical and detection device for light components in residual oil, characterized in that, The device includes: The purge and trap module is used to purge the residual oil sample to be tested in the purge and trap sampler and to capture the light components purged from the residual oil sample through the trap. The desorption module is used to desorb the light components in the residual oil sample to be tested captured by the trap and introduce them into the gas chromatography-mass spectrometry instrument. The analysis and detection module is used to perform qualitative analysis and detection of light components in the desorbed residual oil sample using gas chromatography-mass spectrometry.
9. An electronic device, characterized in that, The electronic device includes: One or more processors; Storage device for storing one or more programs. When the one or more programs are executed by the one or more processors, the one or more processors implement the analytical detection method for light components in residual oil as described in any one of claims 1-7.
10. A storage medium containing computer-executable instructions, characterized in that, The computer-executable instructions, when executed by a computer processor, are used to perform the analytical detection method for light components in residual oil as described in any one of claims 1-7.
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