System and method for determining distillation characteristics of petroleum samples by fractional distillation

Abstract

The apparatus may include a memory storing instructions and a processor configured to execute the instructions to determine an initial mass of the sample, distill the sample to at least a thermal destruction temperature, record vapor temperature values, liquid temperature values, and vapor pressure values ​​associated with the sample at a set of time points during the distillation, and determine a residual mass of the sample. The processor may be further configured to generate a pressure curve based on the vapor pressure values, calculate a summary integral surface of the generated pressure curve, and generate a distillation curve relating the vapor temperature values ​​and liquid temperature values ​​to a mass percentage of the sample evaporated based on the calculated summary integral surface, the initial mass of the sample, and the residual mass of the sample.

Description

[Background technology]

[0001] Petroleum products are used as a fuel source in combustion engines. Different types of petroleum products have different components that exhibit different characteristics. Therefore, the different components can affect the performance of the petroleum product. A distillation process can be performed on a petroleum sample to determine various properties of the sample. Performing a distillation process and characterizing the results of the distillation process can pose various challenges. [Brief explanation of the drawings]

[0002] [Figure 1A] FIG. 1 illustrates a distillation apparatus according to embodiments described herein. [Figure 1B] FIG. 1 shows a distillation apparatus according to another embodiment described herein. [Figure 2] FIG. 2 illustrates exemplary components of a controller unit according to implementations described herein. [Figure 3] FIG. 2 illustrates exemplary functional components of a controller unit according to implementations described herein. [Figure 4] FIG. 1 illustrates exemplary components of a distillation curve database according to implementations described herein. [Figure 5] 1 is a process flow chart for performing distillation according to embodiments described herein. [Figure 6] 1 is a flow chart of a process for analyzing the results of a distillation according to embodiments described herein. [Figure 7] FIG. 1 illustrates an exemplary plot of distillation data according to implementations described herein. [Figure 8] FIG. 1 shows an exemplary distillation curve according to embodiments described herein. DETAILED DESCRIPTION OF THE INVENTION

[0003] The following detailed description refers to the accompanying drawings, in which the same reference numbers in different drawings identify the same or similar elements.

[0004] The distillation apparatus can be used to perform automated distillation of a petroleum sample. Data obtained during the distillation of the petroleum sample can be used to generate a distillation curve that relates one or more properties of the petroleum sample to the temperature during distillation. The distillation curve can then be used to select a safe and reliable mode of transportation and storage and / or to optimize a refining process for a product associated with the petroleum sample.

[0005] The petroleum sample may be placed in a distillation flask and heated to its incipient boiling point. Sensors may monitor the temperature and pressure of the vapor and the temperature of the liquid. Heating of the sample may continue until the sample boils off or until some other end point is reached. One such end point may be the thermal destruction of the sample. Thus, the end distillation temperature may be higher than the sample's thermal destruction temperature. The petroleum sample's thermal destruction temperature may correspond to the temperature at which hydrocarbons or other components of the petroleum sample begin to undergo chemical decomposition through chemical reactions such as oxidation, depolymerization, chain scission, side-chain elimination, and / or other types of chemical reactions that change the petroleum sample's component composition.

[0006] One method for analyzing the distillation characteristics of heavy petroleum samples with final distillation temperatures higher than the thermal breakdown temperature is to mix the heavy petroleum sample with a solvent and distill the mixture. The distillation curve for the heavy petroleum sample can then be extracted from the data by comparing the resulting distillation curve with that of the pure solvent. However, such a procedure is difficult and time-consuming for an operator to perform.

[0007] Embodiments described herein relate to the partial distillation of a petroleum sample having a final distillation temperature greater than its thermal breakdown temperature. For example, the petroleum sample may include crude oil or another heavy petroleum product having a thermal breakdown temperature of about 400° C. Additionally, measurements collected during the distillation may be used to generate a distillation curve relating temperature to the mass percentage of the sample that distilled to that temperature. In order to determine the mass percentage of the sample, information about the mass of the sample may need to be obtained and used in generating the distillation curve.

[0008] Embodiments described herein relate to a distillation apparatus including a mass sensor for determining the mass of a petroleum sample during distillation. In some embodiments, the mass sensor may be attached to an interior wall of the distillation apparatus. In other embodiments, the mass sensor may be external to the distillation apparatus enclosure, for example, attached to an exterior wall of the distillation apparatus.

[0009]

[0003] Embodiments described herein further relate to a method for determining an initial mass and a residual mass of a petroleum sample during distillation and using the initial mass and residual mass to determine the mass percentage of the sample at a particular time during the distillation. The method may include determining the initial mass of the sample, distilling the sample to at least a thermal destruction temperature, recording a set of vapor temperature values, a set of liquid temperature values, and a set of vapor pressure values associated with the sample at a set of time points during the distillation, and determining the residual mass of the sample. The temperature and pressure values may be used to determine physical properties of the sample, such as liquid density and / or vapor density. The method may further include generating a pressure curve based on the set of vapor pressure values, calculating a summary integral surface of the generated pressure curve, and generating a distillation curve relating the set of vapor temperature values and the set of liquid temperature values to the mass percentage of the sample based on the calculated summary integral surface, the initial mass of the sample, and the residual mass of the sample.

[0010] Determining the first moment of boiling may be required to generate an accurate pressure curve. Embodiments described herein further relate to determining the first moment of boiling during the distillation of a petroleum sample, determining the last moment of boiling of the petroleum sample, and generating a pressure curve from the first moment of boiling to the last moment of boiling. In some embodiments, determining the first moment of boiling may include identifying a time point during the distillation at which the vapor pressure value increases above a vapor pressure value typical of the zero line, for example, by identifying a time point at which the vapor pressure value is greater than the highest value of a set of vapor pressure values designated as zero line values by at least a threshold amount.

[0011] In other embodiments, determining the first moment of boiling may include identifying a time point during the distillation at which the vapor pressure noise value increases above a vapor pressure value typical of the zero line, for example, by identifying a time point at which the vapor pressure noise value is greater than the highest value of a set of vapor pressure values designated as zero line values by at least a threshold amount. In yet other embodiments, determining the first moment of boiling includes identifying a time point associated with the first positive extremum in the first derivative of the vapor temperature with respect to time, or the first positive extremum in the second derivative of the vapor temperature with respect to time, or the first negative extremum in the second derivative of the liquid temperature with respect to time.

[0012] In some embodiments, determining the last moment of boiling may include detecting a temperature fluctuation greater than a fluctuation threshold and determining that thermal breakdown has been reached based on detecting a temperature fluctuation greater than the fluctuation threshold.

[0013] Generating the distillation curve may include calculating, for each time point, a ratio of the calculated summary integral surface of the generated pressure curve to the summary integral surface of the generated pressure curve up to that time point multiplied by the ratio of the difference between the initial mass of the sample and the residual mass of the sample to the initial mass of the sample. In some embodiments, the distillation curve may be extrapolated using an extrapolation method to generate a complete distillation curve.

[0014] 1A illustrates a distillation apparatus 101 according to embodiments described herein. The distillation apparatus 101 illustrates an embodiment having a mass sensor 125 attached to a sidewall of the distillation apparatus 101. As shown in FIG. 1A, the distillation apparatus 101 can include a distillation vessel 110, a support 120, a mass sensor 125, a heating element 130, a condenser 145, a vapor temperature sensor 150, a liquid temperature sensor 160, a pressure sensor 170, a controller unit 180, and a fan 185.

[0015] The distillation vessel 110 may include a glass flask having a spherical shape for receiving a sample 112, such as a liquid petroleum sample. The distillation vessel may include a cylindrical neck with a side outlet tube 114, a capillary tube 115 inside the outlet tube 114 and configured to attach to a condenser 145, and a cap 116 configured to seal the distillation vessel 110. In some embodiments, the distillation vessel 110 may be sized to receive 5 to 15 milliliters (ml) of the sample 112 to be analyzed by distillation. In other embodiments, the distillation vessel 110 may be sized to receive different volumes of sample.

[0016] The support 120 may include structural support for the distillation vessel 110, the mass sensor 125, and the heating element 130. In some embodiments, the mass sensor 125 may include a load cell, such as a strain gauge load cell, a piezoelectric load cell, a capacitive load cell, and / or another type of load cell that converts mechanical compression into an electrical signal. In other embodiments, the mass sensor 125 may include a different type of mass sensor, such as a microbalance. The heating element 130 may include a resistive heating element (or another type of heating element, such as a gas source and flame) for applying a controllable heat source to the sample 112. In some embodiments, the mass sensor 125 may be configured to measure the mass of the distillation vessel 110 with the sample 112 and cap 116, as well as the heating element 130. In other embodiments, the distillation vessel 110 may be supported separately from the heating element 130 and attached to the support 120 (e.g., the wall of the distillation apparatus 101) via the mass sensor 125. Thus, heating of the distillation vessel 110 may be performed by heating the internal sealed space of the distillation apparatus 101, and the mass sensor 125 may measure the mass of the distillation vessel 110 with the sample 112 without including the mass of the heating element 130 in the measurement.

[0017] Capillary tube 115 may include tubing (e.g., stainless steel tubing, etc.) inside outlet tube 114 to accept vapors during distillation. Capillary tube 115 may allow for the creation of overpressure within distillation vessel 110 during distillation with gas stream 140. Condenser 145 may include tubing cooled by air cooling, liquid cooling, thermoelectric cooling (e.g., using a Peltier module, etc.), and / or another type of cooling process during distillation to condense distilled vapors from sample 112 into a collection receptacle (not shown in FIG. 1 ).

[0018] The vapor temperature sensor 150 may include an inert temperature sensor, such as, for example, a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or another type of temperature sensor. The vapor temperature sensor 150 is inserted into the neck of the distillation vessel 110 through an opening in the cap 116 to measure the vapor temperature of the sample 112 during distillation.

[0019] The liquid temperature sensor 160 may include, for example, an inert temperature sensor such as a thermocouple, a resistance temperature sensor, a thermistor temperature sensor, a semiconductor temperature sensor, and / or another type of temperature sensor. The liquid temperature sensor 160 may be inserted into the distillation vessel 110 through an opening in the cap 116 to the bottom of the bulb of the distillation vessel 110 and immersed in the sample 112 to measure the liquid temperature of the sample 112 during distillation.

[0020] Pressure sensor 170 may include a pressure sensor for measuring the vapor pressure within distillation vessel 110 during distillation. Pressure sensor 170 may measure the overpressure within distillation vessel 110 during distillation due to the passage of vapor through outlet tube 114, rather than the equilibrium pressure of the vapor within distillation vessel 110. In some embodiments, pressure sensor 170 may include a differential pressure sensor, such as a diaphragm with a piezo-resistive, piezoelectric, and / or capacitive strain gauge. In other embodiments, pressure sensor 170 may include another type of pressure sensor, such as an absolute pressure sensor. During distillation, gas flow 140 is applied to the neck of distillation vessel 110 to protect pressure sensor 170 from high-temperature vapor. Gas flow 140 may be supplied via a micro-compressor (not shown in FIG. 1 ) controlled by controller unit 180 and may include ambient air, an inert gas, and / or another type of gas. For example, the use of an inert gas may increase the maximum possible measured temperature before thermal breakdown occurs due to reduced oxidation of the vapor within distillation vessel 110. The gas flow 140 provides a constant pressure during distillation that must be taken into account to determine the actual pressure of the vapor. The pressure in the distillation vessel 110 may correspond to an overpressure relative to ambient pressure resulting from the vapor passing through the constricted opening of the capillary tube 115. Therefore, the measured vapor pressure may depend not only on the equilibrium vapor pressure of the evaporated sample 112 at a particular temperature, but also on the intensity of the heating and the restricted flow through the capillary tube 115. The actual pressure of the vapor is therefore determined by subtracting the zero-line pressure value from the measured pressure.

[0021] The controller unit 180 may include a processor, microcontroller, and / or computer device that controls the operation of the distillation vessel 110, collects measurements during the distillation, and generates a distillation curve based on the collected measurements. An example configuration of the controller unit 180 is described below with reference to Figures 2 and 3. The fan 185 may be operated at the end of the distillation to cool the distillation vessel 110 after the distillation of the sample 112 is complete.

[0022] 1B illustrates a distillation apparatus 102 according to another embodiment described herein. The distillation apparatus 102 illustrates an embodiment in which the mass sensor 125 is external to the enclosure 122 of the distillation apparatus 102. For example, the mass sensor 125 may be attached to the outer wall of the enclosure 122.

[0023] 1B, distillation apparatus 102 may include distillation vessel 110, enclosure 122, mass sensor 125, heating element 130, condenser 145, vapor temperature sensor 150, liquid temperature sensor 160, pressure sensor 170, controller unit 180, and fan 185. Enclosure 122 may enclose heating element 130 and support and / or may partially enclose distillation vessel 110. Heating element 130, condenser 145, vapor temperature sensor 150, liquid temperature sensor 160, pressure sensor 170, controller unit 180, and / or fan 185 may function as described above with reference to FIG. 1A.

[0024] The mass sensor 125 may include a vessel support 126 for supporting the distillation vessel 110 while the mass of the sample 112 is being measured. The mass of the sample 112 may be measured by placing the distillation vessel 110 with the sample 112 on the vessel support 126 before distillation to measure the initial mass, placing it on the heating element 130 to perform the distillation, and then returning it to the vessel support 126 after distillation to measure the residual mass of the sample 112 after distillation.

[0025] While the distillation apparatus 101 of FIG. 1A may allow for measurement of the mass of the sample 112 while the distillation vessel 110 is in position for distillation and may not require movement of the distillation vessel 110 to measure the initial and residual masses of the sample 112, the distillation apparatus 101 may require a more complex construction. The distillation apparatus 102 of FIG. 1B may require movement of the distillation vessel 110 before and / or after distillation to measure the mass of the sample 112, but may allow for easier construction of the distillation apparatus 102. FIGS. 1A and 1B show exemplary components of the distillation apparatuses 101 and 102; in other embodiments, the distillation apparatuses 101 and / or 102 may include fewer components, different components, components in a different arrangement, or additional components than those shown in FIGS. 1A and 1B. Additionally or alternatively, one or more components of the distillation apparatus 101 and / or 102 may perform functions described as being performed by one or more other components of the distillation apparatus 101 and / or 102.

[0026] 2 is a diagram illustrating exemplary components of a controller unit 180 according to embodiments described herein. As shown in FIG. 2, the controller unit 180 may include a bus 210, a processor 220, a memory 230, an input device 240, an output device 250, and a communication interface 260.

[0027] Bus 210 may include a path that allows communication between components of device 200. Processor 220 may include any type of single-core processor, multi-core processor, microprocessor, latch-based processor, and / or processing logic (or family of processors, microprocessors, and / or processing logic) that interprets and executes instructions. In other embodiments, processor 220 may include an application-specific integrated circuit (ASIC), a field-programmable gate array (FPGA), and / or another type of integrated circuit or processing logic.

[0028] Memory 230 may include any type of dynamic storage device capable of storing information and / or instructions for execution by processor 220, and / or any type of non-volatile storage device capable of storing information for use by processor 220. For example, memory 230 may include random access memory (RAM) or another type of dynamic storage device, read-only memory (ROM) device or another type of static storage device, content addressable memory (CAM), magnetic and / or optical recording memory devices and their corresponding drives (e.g., hard disk drives, optical drives, etc.), and / or removable forms of memory such as flash memory.

[0029] Input device 240 may allow an operator to input information into device 200. Input device 240 may include, for example, a keyboard, a mouse, a pen, a microphone, a remote control, an audio capture device, an image and / or video capture device, a touchscreen display, and / or another type of input device. In some embodiments, device 200 may be remotely administered and may not include input device 240. In other words, device 200 may be "headless," e.g., may not include a keyboard.

[0030] Output device 250 may output information to an operator of device 200. Output device 250 may include a display, a printer, a speaker, and / or another type of output device. For example, device 200 may include a display, which may include a liquid crystal display (LCD), a light emitting diode (LED) display, etc., for displaying content to an operator. In some embodiments, device 200 may be remotely managed and may not include output device 250. In other words, device 200 may be “headless,” e.g., may not include a display.

[0031] The communication interface 260 may include a transceiver that enables the device 200 to communicate with other devices and / or systems via wireless communication (e.g., radio frequency, infrared, and / or optical), wired communication (e.g., conductor, twisted pair cable, coaxial cable, transmission line, fiber optic cable, and / or waveguide, etc.), or a combination of wireless and wired communication. The communication interface 260 may include a transmitter that converts baseband signals to radio frequency (RF) signals and / or a receiver that converts RF signals to baseband signals. The communication interface 260 may be coupled to an antenna for transmitting and receiving RF signals.

[0032] Communications interface 260 may include logical components including input and / or output ports, input and / or output systems, and / or other input and output components that facilitate the transmission of data to other devices. For example, communications interface 260 may include a network interface card (e.g., an Ethernet card) for wired communications and / or a wireless network interface (e.g., WiFi) card for wireless communications. Communications interface 260 may also include a universal serial bus (USB) port for communications over a cable, a Bluetooth™ wireless interface, a radio frequency identification (RFID) interface, a near field communication (NFC) wireless interface, and / or any other type of interface that converts data from one form to another.

[0033] As described in detail below, the apparatus 200 may perform certain operations related to performing a distillation process and generating a distillation curve based on the results of the distillation process. The apparatus 200 may perform these operations in response to the processor 220 executing software instructions contained in a computer-readable medium, such as memory 230. A computer-readable medium may be defined as a non-transitory memory device. The memory device may be implemented in a single physical memory device or distributed across multiple physical memory devices. The software instructions may be loaded into the memory 230 from another computer-readable medium or another device. The software instructions contained in the memory 230 may cause the processor 220 to perform the processes described herein. Alternatively, hardware circuitry may be used in place of or in combination with software instructions to implement the processes described herein. Therefore, the implementations described herein are not limited to any specific combination of hardware circuitry and software.

[0034] 2 illustrates exemplary components of controller unit 180, in other implementations, controller unit 180 may include fewer, different, additional, or differently arranged components than those illustrated in FIGURE 2. Additionally or alternatively, one or more components of controller unit 180 may perform one or more tasks described as being performed by one or more other components of controller unit 180.

[0035] 3 illustrates exemplary functional components of controller unit 180. The functional components of controller unit 180 may be implemented, for example, via processor 220 executing instructions from memory 230. As shown in FIG. 3, controller unit 180 may include a distillation manager 310, a heating element controller 320, a data collector 330, a distillation curve generator 340, a distillation curve database (DB) 350, and a user interface 360.

[0036] Distillation manager 310 may manage the distillation process of distillation apparatus 101 or 102. For example, distillation manager 310 may initiate distillation based on a request from a user received via user interface 360 via heating element controller 320. Heating element controller 320 may control heating element 130. Distillation manager 310 may acquire distillation data using data collector 330, generate a distillation curve using distillation curve generator 340, and provide the generated distillation curve to a user via user interface 360.

[0037] Data collector 330 may manage the collection of data during distillation. Data collector 330 may include a mass sensor controller 332, a vapor temperature sensor controller 334, a liquid temperature sensor controller 336, and a pressure sensor controller 338. Mass sensor controller 332 may control mass sensor 125. Vapor temperature sensor controller 334 may control vapor temperature sensor 150. Liquid temperature sensor controller 336 may control liquid temperature sensor 160. Pressure sensor controller 338 may control pressure sensor 170.

[0038] The distillation curve generator 340 may generate a distillation curve based on data acquired from the data collector 330 and stored in the distillation curve DB 350. An example of information that may be stored in the distillation curve DB 350 is described below with reference to FIG. 4. The distillation curve generator 340 may determine the first and last moments of boiling from the distillation data and generate a pressure curve from the first moment of boiling to the last moment of boiling using a set of pressure values included in the distillation data. The distillation curve generator 340 may then calculate the total summarized integral surface of the generated pressure curve and multiply it by the ratio of the difference between the initial mass of the sample and the residual mass of the sample to the initial mass of the sample to calculate, for each time point, the ratio of the summarized integral surface up to that time point to the total summarized integral surface, thereby generating the mass percentage of the sample distilled up to that time point. The distillation curve generator 340 may then generate a distillation curve relating temperature to mass percentage. In some embodiments, the distillation curve generator 340 may extrapolate the distillation curve to generate a complete distillation curve using an extrapolation method.

[0039] User interface 360 may include a user interface that allows a user to control distillation apparatus 101 or 102 and / or receive information generated by controller unit 180, such as generated distillation curves, messages regarding completed or ongoing distillation processes, and / or other types of messages. User interface 360 may be configured to interact with input device(s) 240 and / or output device(s) 250.

[0040] 3 illustrates exemplary components of controller unit 180, in other implementations, controller unit 180 may include fewer, different, additional, or differently arranged components than those illustrated in FIG. 3. Additionally or alternatively, one or more components of controller unit 180 may perform one or more tasks described as being performed by one or more other components of controller unit 180.

[0041] 4 shows exemplary components of distillation curve DB 350. As shown in FIG. 4, distillation curve DB 350 may include one or more distillation records 400. Each distillation record 400 may store information about a particular distillation performed using distillation apparatus 101 or 102. Distillation record 400 may include a sample identification (ID) field 410, an initial mass field 420, a residual mass field 430, and a distillation data table 440.

[0042] The sample ID field 410 may store an ID associated with the distillation. The initial mass field 420 may store an initial mass associated with the distillation sample (e.g., sample 112). The residual mass field 430 may store a residual mass associated with the distillation sample. The distillation data table 440 may store distillation data associated with the distillation of the sample. The distillation data table 440 may include a set of time point entries 440. Each time point entry 440 may store information about a particular time point during the distillation.

[0043] For example, a time point entry 440 may include a time field 442, a vapor temperature field 444, a liquid temperature field 446, a measured pressure field 448, an actual pressure field 450, a density field 452, a summary surface field 454, and a mass percentage field 456. The time field 442 may store information identifying a particular time point. The vapor temperature field 444 may store a vapor temperature value associated with a particular time point. The liquid temperature field 446 may store a liquid temperature value associated with a particular time point. The measured pressure field 448 may store a measured vapor pressure value associated with a particular time point. The measured vapor pressure value may correspond to the overpressure within the distillation vessel 110 during distillation due to vapor passing through the outlet tube 114. The actual pressure field 450 may store an actual vapor pressure field associated with a particular time point and calculated by taking the difference between the measured pressure field associated with the particular time point and the ambient pressure within the distillation vessel 110 with the gas flow 140.

[0044] The density field 452 may contain a calculated vapor density value associated with a particular point in time. The summary surface field 454 may store a calculated summary integral surface value for a particular point in time. The mass percentage field 456 may store a calculated mass percentage value for a particular point in time.

[0045] Although FIG. 4 illustrates exemplary components of a distillation curve DB 350, in other embodiments, the distillation curve DB 350 may include fewer components, different components, additional components, or components in a different arrangement than those illustrated in FIG. 4.

[0046] Figure 5 is a flow chart of a process 500 for performing distillation according to embodiments described herein. In some embodiments, the process of Figure 5 may be performed by and / or using distillation apparatus 101 or 102. In other embodiments, some or all of the process of Figure 5 may be performed by or using another apparatus or group of apparatuses separate from distillation apparatus 101 and / or 102.

[0047] 5, process 500 may include determining an initial mass of the sample (block 510). For example, controller unit 180 may record the initial mass of sample 112 using mass sensor 125 after sample 112 is placed in distillation vessel 110. Process 500 may further include initiating distillation of the sample (block 520), recording vapor temperature, liquid temperature, and vapor pressure values at each of a set of time points during distillation (block 530), and distilling the sample to at least a thermal destruction temperature (block 540). For example, controller unit 180 may initiate gas flow 140 and then begin heating distillation vessel 110 using heating element 130. Controller unit 180 may obtain the vapor temperature, liquid temperature, and vapor pressure values using vapor temperature sensor 150, liquid temperature sensor 160, and pressure sensor 170, respectively.

[0048] Distillation may continue until a thermal destruction temperature is reached. In some embodiments, thermal destruction may be determined by visual inspection by an operator. For example, the operator may observe the distillation vessel 110 for a change in color of the vapor being distilled, a change observed in the sample 112, etc. In other embodiments, thermal destruction may be automatically detected by the controller unit 180 based on temperature fluctuations. For example, once the thermal destruction temperature is reached, the vapor temperature and / or liquid temperature may stop increasing and begin to fluctuate. The controller unit 180 may be configured to detect a fluctuation in the vapor temperature and / or liquid temperature greater than a fluctuation threshold and stop the distillation by ceasing heating the distillation vessel 110. The controller unit 180 may also activate a fan 185 to cool the distillation vessel 110 at the end of the distillation.

[0049] Process 500 may further include measuring the remaining mass of the sample (block 550). For example, controller unit 180 may record the remaining mass of sample 112 using mass sensor 125 after distillation has stopped. Additionally, process 500 may include generating a distillation curve (block 560) based on the initial mass, the remaining mass, and the recorded sets of vapor temperature, liquid temperature, and vapor pressure values. An exemplary process for generating a distillation curve is described below with reference to FIG. 6.

[0050] Figure 6 is a flow chart of a process for analyzing the results of distillation according to embodiments described herein. In some embodiments, the process of Figure 6 may be performed by and / or using distillation apparatus 101 or 102. In other embodiments, some or all of the process of Figure 6 may be performed by or using another apparatus or group of apparatuses separate from distillation apparatus 101 or 102.

[0051] As shown in FIG. 6 , process 600 may include determining the first moment of boiling (block 610), determining the last moment of boiling (block 620), and generating a pressure curve from the first moment of boiling to the last moment of boiling (block 630). In some embodiments, determining the first moment of boiling may include identifying a time point during the distillation at which the vapor pressure value increases above a vapor pressure value typical of the zero line, for example, by identifying a time point at which the vapor pressure value is greater than the highest value of a set of vapor pressure values designated as a zero line value by at least a threshold amount. The zero line in the data may be established, for example, by identifying data points associated with a slope within a specified range of the zero slope line and / or by using another technique.

[0052] In other embodiments, determining the first moment of boiling may include identifying a time point during the distillation when the vapor pressure noise value increases above a vapor pressure value typical of the zero line, for example, by identifying a time point when the vapor pressure noise value is greater than the highest value of a set of vapor pressure values designated as zero line values by at least a threshold amount. In yet other embodiments, determining the first moment of boiling may include identifying a time point associated with a sudden increase in vapor temperature. A sudden increase in vapor temperature is determined by a relationship between the vapor temperature T with respect to time t. 蒸気 The first positive extremum of the first derivative of

number

number

number

[0053] In some embodiments, determining the last moment of boiling may include detecting a temperature fluctuation greater than a fluctuation threshold and determining that thermal breakdown has been reached based on detecting a temperature fluctuation greater than the fluctuation threshold.

[0054] The process 600 may further include calculating a total summary integral surface of the generated pressure curve (block 640) and, for each time point, calculating a ratio of the total summary integral surface of the generated pressure curve to the summary integral surface up to the time point by multiplying by the ratio of the difference between the initial mass and the residual mass to the initial mass (block 650). For example, the controller unit 180 may calculate a total summary integral surface SS under the pressure curve, defined as m can be calculated.

number

number

[0055] Process 600 may further include generating a distillation curve relating temperature to the mass percentage of the evaporated sample based on the calculated ratio (block 660). For example, controller unit 180 may generate a distillation curve for each time point i by relating the calculated mass % at time point i to the vapor temperature and liquid temperature at time point i.

[0056] 7 illustrates an exemplary plot 700 of distillation data according to embodiments described herein. As shown in FIG. 7, plot 700 illustrates the vapor temperature values (T 蒸気 ) plot, liquid temperature values (T 液体 ) plot, and vapor pressure values (P 蒸気) Plot 700 shows the initial moment 710 of boiling, when the vapor pressure value begins to rise above the zero line by at least a threshold amount. Additionally, plot 700 shows the final moment 720 of boiling, when the vapor temperature and liquid temperature values begin to drop after the onset of thermal breakdown.

[0057] 8 illustrates an exemplary distillation curve 800 according to embodiments described herein. As shown in FIG. 8, a distillation curve represents the mass percentage of a sample that vaporizes at a particular temperature. The distillation curve 800 represents the vapor temperature value (T 蒸気 ), as well as the liquid temperature values (T 液体 ) is shown. As shown in FIG. 8, upon reaching the thermal breakdown temperature, approximately 60% of the sample boils off or is vaporized, generating a partial distillation curve. In some embodiments, the partial distillation curve may be extrapolated to generate a full distillation curve using an extrapolation technique, such as, for example, the Riazi distribution model extrapolation, which uses the determined first moment of boiling and parameters determined from the distillation curve using linear regression. Another extrapolation method that may be used is the Dimudu, Zharkova, and Abayev model of fractional distillation of petroleum products, which uses the first moment of boiling, the last moment of boiling, and a set of coefficients that characterize the distribution of components in the sample. The partial and / or full distillation curves may be used to optimize refining processes and / or to select safe transportation and / or storage modes, etc.

[0058] In the foregoing specification, various preferred embodiments have been described with reference to the accompanying drawings. However, it will be apparent that various modifications and changes may be made and additional embodiments may be implemented without departing from the broader scope of the invention as set forth in the appended claims. Accordingly, the specification and drawings should be regarded in an illustrative rather than a restrictive sense.

[0059] For example, although a series of blocks are described with reference to Figures 5 and 6, the order of the blocks may be changed in other implementations. Furthermore, non-dependent blocks and / or signals may be executed in parallel.

[0060] It will be apparent that the systems and / or methods as described above may be implemented in many different forms of software, firmware, and hardware in the embodiments illustrated in the figures. The actual software code or specialized control hardware used to implement these systems and methods is not limiting of the embodiments. Thus, the operation and behavior of the systems and methods are described without reference to specific software code, and it will be understood that software and control hardware can be designed to implement the systems and methods based on the description herein.

[0061] Furthermore, certain portions described above may be implemented as components that perform one or more functions. A component as used herein may include hardware, such as a processor, ASIC, or FPGA, or a combination of hardware and software (e.g., a processor running software).

[0062] It should be emphasized that as used in this specification, the term "comprises" / "comprising" is to be interpreted as specifying the presence of stated features, integers, steps or components, but does not exclude the presence or addition of one or more other features, integers, steps, components or groups thereof.

[0063] As used herein, the term "logic" may refer to a combination of one or more processors configured to execute instructions stored in one or more memory devices, may refer to hardwired circuitry, and / or may refer to a combination thereof. Furthermore, logic may be contained in a single device or distributed across multiple, possibly remote, devices.

[0064] It is further noted that for purposes of describing and defining the present invention, the term "substantially" is utilized herein to represent the inherent degree of uncertainty that may result from any quantitative comparison, value, measurement, or other representation. The term "substantially" is also utilized herein to represent the extent to which a quantitative representation may vary from the stated standard without resulting in a change in the basic functionality of the subject matter at issue.

[0065] No element, act, or instruction used in the present application should be construed as critical or essential to an embodiment unless explicitly described as such. Also, as used herein, the article "a" is intended to include one or more items. Furthermore, the phrase "based on" is intended to mean "based, at least in part on," unless otherwise specified.

Claims

1. determining an initial mass of the sample; distilling the sample to at least a thermal destruction temperature; recording a plurality of vapor temperature values, a plurality of liquid temperature values, and a plurality of vapor pressure values associated with the sample at a plurality of times during the distillation; determining the residual mass of the sample; generating a pressure curve based on the plurality of vapor pressure values; calculating a summary integral surface of the generated pressure curve; generating a distillation curve relating the plurality of vapor temperature values and the plurality of liquid temperature values to the mass percentage of the sample evaporated based on the calculated summary integral surface, the initial mass of the sample, and the residual mass of the sample; A method comprising:

2. said step of calculating a summary integral surface of said generated pressure curve comprising: determining the first moment of boiling of the sample; determining the last moment of boiling of the sample; generating said pressure curve from the first moment of boiling to the last moment of boiling; The method of claim 1 , comprising:

3. determining the first moment of boiling of the sample; identifying a time point among the plurality of time points associated with a vapor pressure value among the plurality of vapor pressure values that is greater than the highest of a set of vapor pressure values designated as a zero line value by at least a threshold amount; The method of claim 2 , comprising:

4. determining the first moment of boiling of the sample; identifying a time point among the plurality of time points associated with a vapor pressure noise value among the plurality of vapor pressure values that is greater than the highest of a set of vapor pressure values designated as a zero line value by at least a threshold amount; The method of claim 2 , comprising:

5. determining the first moment of boiling of the sample; identifying a time point among the plurality of time points associated with a steam temperature value among the plurality of steam temperature values that is associated with a first positive extremum in a first derivative of the steam temperature with respect to time or a first positive extremum in a second derivative of the steam temperature with respect to time; or identifying a time point among the plurality of time points associated with a liquid temperature value among the plurality of liquid temperature values that is associated with a first negative extremum of a second derivative of the liquid temperature with respect to time; The method of claim 2 , comprising at least one of:

6. detecting a temperature fluctuation greater than a fluctuation threshold; determining that the thermal destruction temperature has been reached based on detecting the temperature fluctuation greater than the fluctuation threshold; The method of claim 1 further comprising:

7. generating the distillation curve comprises: calculating a ratio of the calculated summary integral surface of the generated pressure curve for a particular point in time among the plurality of points in time to the summary integral surface of the generated pressure curve up to the particular point in time by multiplying the ratio of the difference between the initial mass of the sample and the residual mass of the sample to the initial mass of the sample; The method of claim 1 , comprising:

8. extrapolating the generated distillation curve to generate a complete distillation curve. The method of claim 1 further comprising:

9. a memory for storing instructions; a processor; An apparatus comprising: The processor executes the instructions to Determine the initial mass of the sample; distilling the sample to at least its thermal destruction temperature; recording a plurality of vapor temperature values, a plurality of liquid temperature values, and a plurality of vapor pressure values associated with the sample at a plurality of time points during the distillation; determining the residual mass of the sample; generating a pressure curve based on the plurality of vapor pressure values; calculating a summary integral surface of the generated pressure curve; generating a distillation curve relating the plurality of vapor temperature values and the plurality of liquid temperature values to the mass percentage of the sample evaporated based on the calculated summary integral surface, the initial mass of the sample, and the residual mass of the sample; It is configured as follows: Device.

10. When calculating the summary integral surface of the generated pressure curve, the processor: determining the first moment of boiling of the sample; determining the last moment of boiling of the sample; generating a pressure curve from the first moment of boiling to the last moment of boiling; The apparatus of claim 9 further configured to:

11. When determining the first moment of boiling of the sample, the processor: identifying a time point among the plurality of time points associated with a vapor pressure value among the plurality of vapor pressure values that is greater than the highest of a set of vapor pressure values designated as a zero line value by at least a threshold amount; The apparatus of claim 10 further configured to:

12. When determining the first moment of boiling of the sample, the processor: identifying a time point among the plurality of time points associated with a vapor pressure noise value among the plurality of vapor pressure values that is greater than the highest of a set of vapor pressure values designated as a zero line value by at least a threshold amount; The apparatus of claim 10 further configured to:

13. When determining the first moment of boiling of the sample, the processor Identifying a time point among the plurality of time points associated with a steam temperature value among the plurality of steam temperature values that is associated with a first positive extremum in a first derivative of the steam temperature with respect to time or a first positive extremum in a second derivative of the steam temperature with respect to time; or Identifying a time point among the plurality of time points associated with a liquid temperature value among the plurality of liquid temperature values that is associated with a first negative extremum of a second derivative of the liquid temperature with respect to time. The apparatus of claim 10 further configured to:

14. When generating the distillation curve, the processor: calculating a ratio of the calculated summary integral surface of the generated pressure curve for a particular time point among the plurality of time points to the summary integral surface of the generated pressure curve up to the particular time point by multiplying the ratio of the difference between the initial mass of the sample and the residual mass of the sample to the initial mass of the sample; The apparatus of claim 9 further configured to:

15. Further comprising a distillation flask; The distillation flask is a mass sensor for determining the initial mass and the residual mass of the sample; a steam temperature sensor for obtaining the plurality of steam temperature values; a liquid temperature sensor for obtaining the plurality of liquid temperature values; a pressure sensor for acquiring the plurality of vapor pressure values; 10. The apparatus of claim 9, comprising:

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