Hydrocarbon measurement device and hydrocarbon composition measurement method

Abstract

The invention provides a hydrocarbon determination device and a hydrocarbon composition determination method. The device comprises a box body and heating devices symmetrically fixed on two sides of the inner wall of the box body, the temperature control box is located above the right side outside the box body, and the heating device is connected with the temperature control box through a signal control line; the temperature control probe is fixed in the box body; the air purification device is located on the upper edge of the interior of the box body, and the air purification device comprises a first exhaust fan; a second exhaust fan is further arranged on the upper edge in the box body; the air speed control box is arranged below the temperature control box, and the air speed control box is connected with the first exhaust fan and the second exhaust fan; the scale is parallel to the analysis column, and the reading module is nested on the scale and slides on the scale along the vertical direction. The hydrocarbon determination device solves the problems of sample solidification caused by low temperature, long test time and reagent volatilization of the existing instrument, and meets the requirements of actual analysis and detection.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection equipment, and in particular to a hydrocarbon determination device and a hydrocarbon composition determination method. Background Art

[0002] Petroleum hydrocarbons are one of the widely existing organic pollutants in the environment, including gasoline, kerosene, diesel, lubricating oil, paraffin and asphalt. They are a mixture of various hydrocarbons (normal alkanes, branched alkanes, cycloalkanes, aromatics) and a small amount of other organic matter.

[0003] With the development of science and technology, inspection technology is changing with each passing day, and advanced inspection instruments are constantly updated. Especially with the improvement of the automation level of instruments and the miniaturization of instruments, the functions of instruments are constantly enhanced. The addition of various automatic detection and automatic control functions makes the instrument more compact and the structure more complex. The hydrocarbon analyzer is an instrument used to determine the volume fraction of aromatic hydrocarbons, olefins and saturated hydrocarbons in petroleum fractions. Its working principle is to take a certain volume of sample and inject it into the activated analytical column. A thin layer of silica gel containing a mixture of fluorescent dyes is installed in the separation section of the adsorption column. When the sample is completely adsorbed on the silica gel, an organic reagent is added to desorb the sample, and the sample is pressurized to flow down the column. The various hydrocarbons in the sample are separated into aromatic hydrocarbons, olefins and saturated hydrocarbons according to their adsorption capacity. The fluorescent dye is also selectively separated from the hydrocarbon instrument, so that the interface of various hydrocarbon regions is clearly visible under ultraviolet light, and the volume fraction of each hydrocarbon is calculated according to the length of each hydrocarbon color band region in the adsorption column.

[0004] At present, the commonly used hydrocarbon measuring instrument in the laboratory is composed of gas system, vibration part, scale and scale indication, system lighting, ultraviolet light detection and other components. It adopts a closed and integrated structure, with two imported precision adsorption columns built in. The instrument is equipped with a cleaning device. After each test, it is not necessary to remove the adsorption column from the instrument. The adsorption column can be cleaned conveniently and quickly on the instrument. The ultraviolet lamp is built-in to avoid harm to the human body, and the hydrocarbon content of liquid petroleum products can be measured safely and accurately.

[0005] However, the temperature is not controlled in the prior art. When the indoor temperature is low, the oil is prone to solidification. After measuring a certain volume of sample and injecting it into a glass analysis column filled with activated silica gel, the sample is easy to condense here, which slows down the separation speed of the sample during the analysis and prolongs the test time, ultimately resulting in low analysis efficiency, high test energy consumption, increased analysis costs, and the separation effect of the sample components seriously affects the accuracy of the test data. Therefore, it is necessary to effectively monitor the temperature to ensure efficient separation of the sample. In addition, organic reagents are used in the process of sample filling and cleaning. The reagents are highly volatile and seriously endanger the health of the operators. Therefore, it is necessary to conduct in-depth research on the issues of sample solidification and safety and environmental protection in order to achieve rapid and accurate determination of the hydrocarbon content in oil products. Summary of the invention

[0006] In view of the deficiencies in the above-mentioned prior art, the present invention provides a hydrocarbon determination device and a hydrocarbon composition determination method. The hydrocarbon determination device solves the problems of sample solidification due to low temperature, long test time, and volatilization of reagents in existing instruments, thereby meeting the needs of actual analysis and detection.

[0007] In order to achieve the above object, the present invention provides a hydrocarbon determination device, comprising:

[0008] A box body, and heating devices symmetrically fixed on both sides of the inner wall of the box body;

[0009] A temperature control box is located on the upper right side of the box body, and the heating device is connected to the temperature control box through a signal control line;

[0010] A temperature control probe is fixed in the box;

[0011] An air purification device is located at the upper edge of the interior of the box, and the air purification device includes a first exhaust fan; a second exhaust fan is also provided at the upper edge of the interior of the box;

[0012] A wind speed control box is arranged below the temperature control box, and the wind speed control box is connected to the first exhaust fan and the second exhaust fan;

[0013] An analysis column and a ruler arranged parallel to the analysis column, wherein the reading module is nested on the ruler and slides on the ruler in a vertical direction.

[0014] In some embodiments, the heating devices located on the same side are distributed up and down.

[0015] In some embodiments, a first fixed thin rod and a second fixed thin rod are symmetrically fixed in the box body, the first fixed thin rod and the second fixed thin rod are fixed to the box body at their upper and lower ends, and the temperature control probe is fixed to the first fixed thin rod and the second fixed thin rod;

[0016] There are two scales, namely a first scale and a second scale. The first scale is arranged in parallel on the left side of the first fixed thin rod, and the second scale is arranged in parallel on the right side of the second fixed thin rod.

[0017] In some embodiments, a first fixing rod and a second fixing rod are symmetrically arranged in the box body, both ends of the first fixing rod and the second fixing rod are fixed to the box body, a first fixing clamp and a first fixing knob are installed on the first fixing rod, and the first fixing knob is used to fix the first ultraviolet lamp, the first analytical column and the first ruler in sequence, and a first reading module is nested on the first ruler;

[0018] A second fixing clamp and a second fixing knob are installed on the second fixing rod, and the second fixing knob is used to fix the second ultraviolet lamp, the second analysis column and the second ruler in sequence. The second reading module is nested on the second ruler, and the first analysis column and the second analysis column are respectively connected to gas pipelines.

[0019] In some embodiments, the number of the second row of fans is two, which are respectively located between the heating device and the first fixing rod, and between the heating device and the second fixing rod.

[0020] In some embodiments, the air purification device is arranged between the first fixed thin rod and the second fixed thin rod, and the air purification device also includes an exhaust hood, an aluminum foil tube and an adsorption module connected in sequence, and the adsorption module includes activated carbon filler, PP cotton filler and composite filler.

[0021] In some of the embodiments, the analytical column is made of a precision inner diameter glass tube or a standard wall glass tube, and the analytical column includes a feeding section, a separation section and an analysis section with a capillary neck; or is made of a standard wall glass tube.

[0022] In some of the embodiments, the hydrocarbon determination device further comprises a control system, and the control system implements operation program control through a control panel, and a pressure gauge, a power control switch and a pressure control switch are installed on the control panel.

[0023] In some embodiments, the first row of fans and the second row of fans can adjust the wind speed, which is divided into first gear, second gear and third gear.

[0024] The present invention also provides a method for determining hydrocarbon composition, which is performed using the above-mentioned hydrocarbon determination device. The method for determining hydrocarbon composition comprises the following steps:

[0025] Turn on the air purification device, adjust the wind speed control box, set the appropriate wind speed, fill the analytical column with filler and dyed silica gel, extract the sample and inject it into the analytical column, add organic reagent, connect the gas pipeline, pressurize the sample to separate in the analytical column, and turn off the air purification device;

[0026] Turn on the exhaust fan, adjust the wind speed control box to set the appropriate wind speed, and adjust the temperature control box to set the temperature to a suitable temperature. At this time, the heating device starts heating. When the temperature control probe detects that the box temperature reaches the set temperature, the heating device automatically stops heating.

[0027] Aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample move from top to bottom of the analytical column, and are repeatedly adsorbed and desorbed on the analytical column, so that the aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample are separated in order of strength on the adsorption column. Fluorescent dyes are also selectively separated together with aromatic hydrocarbons, olefins and saturated hydrocarbons, so that the interface of aromatic hydrocarbons, olefins and saturated hydrocarbons produces red, blue, yellow and colorless spectrum bands under ultraviolet light.

[0028] Turn on the UV lamp, and when the red interface enters the analysis section about 350 mm, move the reading module to calculate the volume percentage of each hydrocarbon based on the area length of the aromatic, olefin and saturated hydrocarbon bands in the analysis column.

[0029] Compared with the prior art, the present invention has the following advantages:

[0030] The hydrocarbon determination device provided by the present invention solves the problem of sample solidification and long test time due to low temperature by arranging a temperature control device on the right side and inside the box, thereby reducing energy consumption, saving resources and lowering economic costs;

[0031] In the hydrocarbon determination device provided by the present invention, a temperature control point is arranged inside the box, and a temperature circulation device is formed through the interaction of multiple thermocouples and exhaust fans, which ensures rapid heating and uniform heating, high heating efficiency, and prevents local overheating from causing sample volatilization and affecting the accuracy of the final test result.

[0032] The hydrocarbon determination device provided by the present invention effectively avoids harm to our living environment and health by adding an air purification device. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0034] Figure 1 It is a schematic diagram of the structure of a hydrocarbon determination device shown in an embodiment of the present invention;

[0035] Figure 2 This is a schematic diagram of the structure of an air purification device according to an embodiment of the present invention;

[0036] Figure 3 This is a schematic diagram of a control system shown in an embodiment of the present invention;

[0037] in:

[0038] 1-Box; 2-Heating device; 3-Temperature control box; 4-Temperature control probe;

[0039] 5-air purification device; 501-first exhaust fan; 502-exhaust hood; 503-aluminum foil tube; 504-adsorption module; 5041-activated carbon filler; 5042-PP cotton filler; 5043-composite filler;

[0040] 6- Second row fan; 7- Wind speed control box;

[0041] 81-first fixed thin rod; 91-first ruler; 101-first fixed rod; 111-first fixed clamp; 121-first fixed knob; 131-first ultraviolet lamp; 141-first analytical column; 151-first reading module;

[0042] 82 - second fixed thin rod; 92 - second scale; 102 - second fixed rod; 112 - second fixed clamp; 122 - second fixed knob; 132 - second ultraviolet lamp; 142 - second analytical column; 152 - second reading module;

[0043] 15- Gas pipeline;

[0044] 16- control panel; 1601- pressure gauge; 1602- power control switch; 1603- pressure control switch. DETAILED DESCRIPTION

[0045] The technical solution of the present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments to further understand the purpose, solution and effect of the present invention, but it is not intended to limit the scope of protection of the claims attached to the present invention.

[0046] Certain words are used in the specification and subsequent claims to refer to specific components or parts. It should be understood by those of ordinary skill in the art that technical users or manufacturers may refer to the same component or part by different nouns or terms. This specification and subsequent claims do not use differences in names as a way to distinguish components or parts, but use differences in the functions of components or parts as the criteria for distinction. "Including" and "comprising" mentioned throughout the specification and subsequent claims are open-ended terms and should be interpreted as "including but not limited to". In addition, the word "connect" here includes any direct and indirect electrical connection means. Indirect electrical connection means include connection through other devices.

[0047] It should be noted that, in the description of the present invention, the terms "lateral", "longitudinal", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and "about", or "approximately", "substantially", "left and right" and the like indicating directions or positional relationships or parameters are all based on the directions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description content, and do not indicate or imply that the referred device or element must have a specific direction, specific size, or be constructed and operated in a specific direction, and therefore cannot be understood as a limitation on the present invention.

[0048] The hydrocarbon measuring instrument is an instrument for measuring the volume fraction of aromatics, olefins and saturated hydrocarbons in petroleum fractions. The measuring method is to use a fluorescent indicator to make the main hydrocarbons in the petroleum product appear on the silica gel adsorption column, and then calculate its volume percentage content. It is suitable for the method specified in GB / T11132 as a quality measurement indicator for fuel oil such as engine fuel and aviation fuel. However, the instrument has the disadvantage that the experimental measurement results are easily affected by the environment, especially the indoor temperature. Temperature is a major controlled parameter in the detection process and a common process variable. When the indoor temperature is low, it is easy to cause the separation speed in the sample analysis process to slow down. Gas, coal and diesel are very likely to solidify, making it difficult to separate the sample in the analytical column, resulting in a long analysis time and high energy consumption, which will not only reduce the analysis efficiency and increase the analysis cost, but also affect the accuracy of the data; in addition, organic reagents are used in the sample filling and cleaning process, and the reagents are highly active, which seriously endangers the health of the operator. In view of this situation, the present invention provides a hydrocarbon measuring device, which has an online heating function and improves the problem of volatilization of reagents in existing instruments to meet the needs of actual analysis and detection.

[0049] See also Figure 1-3The first embodiment of the present invention provides a hydrocarbon determination device, comprising: a box body 1, and heating devices 2 symmetrically fixed on both sides of the inner wall of the box body 1, the heating devices 2 located on the same side are distributed up and down, and preferably, the heating temperature is controlled at 30-35°C; wherein the outer part of the box body 1 is a rectangular parallelepiped structure, and the box body 1 adopts an iron shell and is opaque on all sides. A temperature control box 3 is located on the upper right side outside the box body 1, and the heating device 2 is connected to the temperature control box 3 through a signal control line; a temperature control probe 4 is fixed in the box body 1; an air purification device 5 is located on the upper edge of the inside of the box body 1, and the air purification device 5 includes a first exhaust fan 501; a second exhaust fan 6 is also provided on the upper edge of the inside of the box body 1; a wind speed control box 7 is arranged below the temperature control box 3, and the wind speed control box 7 is connected to the first exhaust fan 501 and the second exhaust fan 6 so as to transfer the heat emitted by the heating device to the inside of the entire box body 1; an analytical column and a scale arranged parallel to the analytical column, and the reading module is nested on the scale and slides on the scale in a vertical direction.

[0050] The temperature control box 3 described in this embodiment is installed on the right side of the outer wall of the box body 1, and is used to control the temperature inside the box body of the hydrocarbon determination device. The temperature control box 3 is a rectangular box body with a temperature display screen and a temperature adjustment button on the surface. A relay is provided on the upper inner wall of the temperature control box 3 to protect the circuit and equipment. When the temperature reaches the set value, it is automatically disconnected. The temperature control box 3 is connected to the temperature control probe 4 through a signal control line. The temperature control probe 4 is fixed on both sides of the fixed rod to sense the temperature inside the box and transmit a signal to the relay when the set value is reached.

[0051] The wind speed control box in this embodiment is installed on the right side of the outer wall of the box body, located below the temperature controller and is used to control the wind speed inside the hydrocarbon measuring device box. The wind speed adjustment control box includes an adjustment control wireless module and a processor connected to the adjustment control wireless module, which is used to adjust the wind speed.

[0052] In this embodiment, a first fixed thin rod 81 and a second fixed thin rod 82 are symmetrically fixed in the box body. The first fixed thin rod 81 and the second fixed thin rod 82 are fixed on the box body 1 at their upper and lower ends, and the temperature control probe 4 is fixed on the first fixed thin rod 81 and the second fixed thin rod 82.

[0053] There are two scales, which are made of alloy material, namely a first scale 91 and a second scale 92 . The first scale 91 is arranged in parallel on the left side of the first fixed thin rod 81 , and the second scale 92 is arranged in parallel on the right side of the second fixed thin rod 82 .

[0054] In the present embodiment, the box body is symmetrically provided with a first fixing rod 101 and a second fixing rod 102, both ends of which are fixed to the box body 1, and the first fixing rod 101 is provided with a first fixing clamp 111 and a first fixing knob 121, and the first fixing knob 121 is used to sequentially fix the first ultraviolet lamp 131, the first analytical column 141 and the first ruler 91, and the first reading module 151 is nested on the first ruler 91;

[0055] A second fixing clamp 112 and a second fixing knob 122 are installed on the second fixing rod 102, and the second fixing knob 122 is used to fix the second ultraviolet lamp 132, the second analysis column 142 and the second scale 92 in sequence. A second reading module 152 is nested on the second scale 92, and the first analysis column 141 and the second analysis column 142 are respectively connected to the gas pipeline 15. It should be known that in this embodiment, the analytical columns are arranged inside the box 1, which can be 2 groups or 4 groups.

[0056] There are two second exhaust fans 6 , which are respectively disposed between the heating device 2 and the first fixing rod 101 , and between the heating device 2 and the second fixing rod 102 .

[0057] The air purification device 5 is arranged between the first fixed thin rod 81 and the second fixed thin rod 82, and is used for air purification when filling samples and cleaning analytical columns. The air purification device 5 also includes an exhaust hood 502, an aluminum foil tube 503 and an adsorption module 504 which are connected in sequence. The adsorption module 504 includes an activated carbon filler 5041, a PP cotton filler 5042 and a composite filler 5043. In this embodiment, the exhaust fan of the air purification device is connected to the wind speed control box through signal transmission. The exhaust hood is connected to the through a connecting device. The connecting device is an aluminum foil tube with a telescopic function, which passes through the box to connect the exhaust hood and the exhaust fan. An exhaust fan is arranged between the connecting device and the adsorption module. The connecting device is connected to the air inlet of the exhaust fan. The air outlet of the exhaust fan is connected to the air inlet of the adsorption module. The exhaust fan can accelerate the air flow in the box and accelerate the purification of the exhaust gas.

[0058] The analytical column in this embodiment is made of a precision inner diameter glass tube or a standard wall glass tube, and includes a feeding section, a separation section and an analysis section with a capillary neck; or is made of a standard wall glass tube; wherein the inner diameter of the analysis section is 1.60mm-1.65mm.

[0059] The hydrocarbon determination device described in this embodiment also includes a control system, which implements operation program control through a control panel 16. The temperature control device, wind speed control device and air purification system prompt the replacement of packing. The control panel 16 is equipped with a pressure gauge 1601, a power control switch 1602 and a pressure control switch 1603.

[0060] Among them, the first row of fans and the second row of fans can adjust the wind speed, which is divided into first gear, second gear and third gear, the first gear is 10-15m / s, the second gear is 15-20m / s, and the third gear is 20-25m / s.

[0061] The hydrocarbon determination device and hydrocarbon composition determination method provided by the present invention have heating devices installed on both sides of the inner wall of the box to provide a heat source for the box; a wind control device and a temperature control device are installed on the outer wall of the box to control the wind speed and temperature in the box of the hydrocarbon determination device, ensuring that the state of the sample is not affected by the temperature during the test, and effectively shortening the test time, greatly improving the analysis efficiency; an air purification device is installed on the upper edge of the inner wall of the box to purify the air when filling samples and cleaning the analysis column, effectively avoiding physical damage to the analysis test personnel during the sample filling process. The present invention has the characteristics of good applicability, high accuracy, and easy operation.

[0062] Another embodiment of the present invention provides a method for measuring hydrocarbon composition, which is performed using the above-mentioned hydrocarbon measuring device. The method for measuring hydrocarbon composition comprises the following steps:

[0063] Open the air purification device 5, adjust the wind speed control box 7, set a suitable wind speed, fill the analytical columns (141, 142) with fillers and dyed silica gel, extract samples and inject them into the analytical columns (141, 142), add organic reagents, connect the gas pipeline 15, pressurize the samples to separate them in the analytical columns, and close the air purification device 5;

[0064] Turn on the exhaust fan 6, adjust the wind speed control box 7, set the appropriate wind speed, and adjust the temperature control box 3 to set the temperature to a suitable temperature. At this time, the heating device 2 starts heating. When the temperature control probe 4 detects that the box temperature reaches the set temperature, the heating device 2 automatically stops heating.

[0065] Aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample move from top to bottom of the analytical column due to differences in their adsorption capacity in the filler, and are repeatedly adsorbed and desorbed on the analytical column, so that the aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample are separated in order of strength on the adsorption column. Fluorescent dyes are also selectively separated together with aromatic hydrocarbons, olefins and saturated hydrocarbons, so that the interface of aromatic hydrocarbons, olefins and saturated hydrocarbons produces red, blue, yellow and colorless bands under ultraviolet light.

[0066] The ultraviolet lamp (131, 132) is turned on, and when the red interface enters the analysis section by about 350 mm, the reading module (151, 152) is moved to calculate the volume percentage of each hydrocarbon based on the area length of the aromatic, olefin and saturated hydrocarbon bands in the analysis column.

[0067] In this embodiment, a UV lamp is installed in the box, and two 915-1220mm long UV lamp tubes are installed vertically and parallel to the adsorption column; the wavelength of the light source is 365nm, and the light source is adjusted to emit the best fluorescence; the silica gel should be activated before use, placed in a shallow container, dried at 175℃-200℃ for 3-4h, and put into a sealed container while hot to avoid moisture; the organic reagent used is isopropanol or isopentanol. When the final distillation range of the sample is less than 204℃, the selected solvent is isopropanol, and when the final distillation range of the sample is greater than 204℃, the selected solvent is isopentanol;

[0068] The pressure regulator in this embodiment can adjust and maintain the pressure delivery range of 0kPa-103kPa, and keep it at 0.5kpa when measuring the sample; the volume of the syringe is 1mL, and the graduation is 0.01mL or 0.02mL; the syringe needle is 100mm long, with an outer diameter of about 1.0mm, and the needle tip is at a certain angle.

[0069] The hydrocarbon determination device and hydrocarbon composition determination method provided by the present invention are applied to determine the volume percentage of saturated hydrocarbons, olefins and aromatic hydrocarbons in liquid petroleum products. In the experiment, an air purification device is turned on, and a fluorescent indicator is used to display the main hydrocarbons in the liquid petroleum products on a silica gel adsorption column. The temperature control device is turned on to maintain the temperature within a specific range, so that the sample can be efficiently separated and its volume percentage can be calculated. The method greatly shortens the analysis time and improves the analysis and detection efficiency.

[0070] The specific examples and comparative examples of using the hydrocarbon determination device of the present invention to determine the hydrocarbon composition of a standard sample are as follows:

[0071] Example 1

[0072] Test instruments and reagents

[0073] Instrument: The hydrocarbon determination device of the present invention.

[0074] Silica gel: Meet the following specifications: Surface area 430-530m 2 / g; pH value of 5% aqueous suspension is 5.5-7.0; 955℃ ignition loss (mass fraction): 4.5-10.0%; iron content (calculated as Fe2O3, dry basis): ≤50mg / kg.

[0075] Determination of pH value: Calibrate the pH meter with standard buffer solutions with pH values ​​of 4 and 7, place 5g of silica gel in a 250mL beaker, add 100mL of water and a stirring rod, stir on a magnetic stirrer for 20 minutes, and then use a calibrated pH meter to determine its pH value. Silica gel should be activated before use, placed in a shallow container, dried at 175°C for 3 hours, and placed in a sealed container while hot to prevent moisture.

[0076] Fluorescent indicator dyed silica gel: Standard dyed silica gel is obtained by recrystallizing Oil Red AB4 and olefin and aromatic dye purification parts obtained by chromatographic adsorption, and depositing them on silica gel through a specific procedure. Dyed silica gel should be stored in a dark place under normal pressure nitrogen, so that the dyed silica gel can have a service life of at least 5 years. It is best to take out a part of the dyed silica gel for daily use and put it in a small bottle to avoid affecting the service life of most of the dyed silica gel due to frequent use.

[0077] Isopropyl alcohol: analytical grade, content not less than 99%.

[0078] Compressed gas: air (or nitrogen), delivered to the top of the adsorption column at a controllable pressure range of 0kPa-103kPa.

[0079] Acetone: analytical grade.

[0080] Petroleum ether: analytical grade.

[0081] Ethanol: analytical grade.

[0082] Buffer solutions: pH values ​​are 4 and 7 respectively.

[0083] Standard sample: Commercially available gasoline standard sample, aromatic content: 35%; olefin content: 20%; saturated hydrocarbon content: 45%.

[0084] Test steps

[0085] 1) Filling with silica gel

[0086] Place a small piece of absorbent cotton between the spherical ground mouth and the spherical socket at the end of the cleaned adsorption column, and clamp it with a small steel clamp. Turn on the vibrator and fill the silica gel while vibrating. When the separation section is half filled, stop vibrating, fill 3-5mm fluorescent indicator, then fill some silica gel, and then start vibrating again, so that the silica gel is filled to 75mm in the feeding section, and then stop vibrating after 4 minutes. Turn on the air purification device. Adjust the wind speed to 10m / s.

[0087] 2) Take samples

[0088] Use a sampler to extract 0.75±0.03ml of standard sample, insert the needle into the silica gel 30mm and inject the sample to allow the sample to be fully adsorbed.

[0089] 3) Inject reagent

[0090] After all the samples are adsorbed, inject isopropanol into the feeding section to the spherical joint, connect the top of the adsorption column to the air supply system, and clamp the spherical ground joint with a clamp.

[0091] 4) Pressurization

[0092] Maintain the pressure at 14kPa±2kPa for 2.5min±0.5min to allow the liquid to move downward along the adsorption column. Then increase the pressure to 34kPa±2kPa and maintain it for another 2.5min±0.5min, and finally adjust the air pressure to an appropriate pressure to allow the liquid to move downward.

[0093] 5) Start the temperature control device and adjust the temperature to 30°C.

[0094] 6) Reading

[0095] When the red alcohol-aromatic interface enters the analysis section about 350mm, quickly mark the interfaces of various hydrocarbons observed under ultraviolet light in the following order (from bottom to top) to measure a set of data. For the non-fluorescent saturated hydrocarbon area, mark the front edge of the sample and the position where the yellow fluorescence first reaches the strongest; for the second part, i.e., the upper end of the olefin area, mark the position where the strong blue fluorescence first appears; for the third part, i.e., the upper end of the aromatic area, mark the upper end of the first red or brown ring.

[0096] 3. Test results

[0097] After the above operation, the area lengths of the aromatic, olefin and saturated hydrocarbon bands were obtained, and the volume percentage of each hydrocarbon was calculated according to formula (1-3). The comparison between the results of the heating condition and the standard sample is shown in Table 1.

[0098] C1=(L1 / L)×100……………………(1)

[0099] C2=(L2 / L)×100……………………(2)

[0100] C3=(L3 / L)×100……………………(3)

[0101] Where: C1—volume fraction of aromatics, %;

[0102] C2—olefin volume fraction, %;

[0103] C3—volume fraction of saturated hydrocarbons, %;

[0104] L1—Aromatic region length, in millimeters (mm);

[0105] L2—olefin region length, in millimeters (mm);

[0106] L3—saturated hydrocarbon region length, in millimeters (mm);

[0107] L—the sum of L1+L2+L3, in millimeters (mm)

[0108] Table 1 Test results of standard samples and actual samples in heating mode

[0109] sample Standard samples first Second time The third time Fourth Fifth Aromatics / %(V / V) 35.0 35.0 35.1 35.2 34.5 35.2 Olefin / %(V / V) 20.0 19.4 19.6 20.5 19.0 20.0 Saturated hydrocarbons / %(V / V) 45.0 45.6 45.3 44.3 46.5 44.8

[0110] Comparative Example 1

[0111] The operation in the comparative example was repeated. The hydrocarbon composition of the diesel sample was measured using the hydrocarbon measuring device of the present invention.

[0112] 1. Test instruments and reagents

[0113] Instrument: The hydrocarbon determination device of the present invention.

[0114] Silica gel: Meet the following specifications: Surface area 430-530m 2 / g; pH value of 5% aqueous suspension is 5.5-7.0; 955℃ ignition loss (mass fraction): 4.5-10.0%; iron content (calculated as Fe2O3, dry basis): ≤50mg / kg.

[0115] Determination of pH value: Calibrate the pH meter with standard buffer solutions with pH values ​​of 4 and 7, place 5g of silica gel in a 250mL beaker, add 100mL of water and a stirring rod, stir on a magnetic stirrer for 20 minutes, and then use a calibrated pH meter to determine its pH value. Silica gel should be activated before use, placed in a shallow container, dried at 175°C for 3 hours, and placed in a sealed container while hot to prevent moisture.

[0116] Fluorescent indicator dyed silica gel: Standard dyed silica gel is obtained by recrystallizing Oil Red AB4 and olefin and aromatic dye purification parts obtained by chromatographic adsorption, and depositing them on silica gel through a specific procedure. Dyed silica gel should be stored in a dark place under normal pressure nitrogen, so that the dyed silica gel can have a service life of at least 5 years. It is best to take out a part of the dyed silica gel for daily use and put it in a small bottle to avoid affecting the service life of most of the dyed silica gel due to frequent use.

[0117] Isoamyl alcohol: analytically pure, content not less than 99%.

[0118] Compressed gas: air (or nitrogen), delivered to the top of the adsorption column at a controllable pressure range of 0kPa-103kPa.

[0119] Buffer solutions: pH values ​​are 4 and 7 respectively.

[0120] Diesel: From a domestic petrochemical plant.

[0121] 2. Test steps

[0122] 1) Filling with silica gel

[0123] Place a small piece of absorbent cotton between the spherical ground mouth and the spherical socket at the end of the cleaned adsorption column, and clamp it with a small steel clamp. Turn on the vibrator and fill the silica gel while vibrating. When the separation section is half filled, stop vibrating, fill 3-5mm fluorescent indicator, then fill some silica gel, and then start vibrating again, so that the silica gel is filled to 75mm in the feeding section, and then stop vibrating after 4 minutes. Turn on the air purification device. Adjust the wind speed to 10m / s.

[0124] 2) Take samples

[0125] Use a sampler to extract 0.75±0.03ml of standard sample, insert the needle into the silica gel 30mm and inject the sample to allow the sample to be fully adsorbed.

[0126] 3) Inject reagent

[0127] After all the samples are adsorbed, inject isopropanol into the feeding section to the spherical joint, connect the top of the adsorption column to the air supply system, and clamp the spherical ground joint with a clamp.

[0128] 4) Pressurization

[0129] Maintain the pressure at 14kPa±2kPa for 2.5min±0.5min to allow the liquid to move downward along the adsorption column. Then increase the pressure to 34kPa±2kPa and maintain it for another 2.5min±0.5min, and finally adjust the air pressure to an appropriate pressure to allow the liquid to move downward.

[0130] 5) Start the temperature control device and adjust the temperature to 30°C.

[0131] 6) Reading

[0132] When the red alcohol-aromatic interface enters the analysis section about 350mm, quickly mark the interfaces of various hydrocarbons observed under ultraviolet light in the following order (from bottom to top) to measure a set of data. For the non-fluorescent saturated hydrocarbon area, mark the front edge of the sample and the position where the yellow fluorescence first reaches the strongest; for the second part, i.e., the upper end of the olefin area, mark the position where the strong blue fluorescence first appears; for the third part, i.e., the upper end of the aromatic area, mark the upper end of the first red or brown ring.

[0133] 3. Test results

[0134] After the above operation, the area lengths of the aromatic, olefin and saturated hydrocarbon bands were obtained, and the volume percentage of each hydrocarbon was calculated according to formula (1-3). The comparison of the results with and without heating is shown in Table 2.

[0135] C1=(L1 / L)×100……………………(1)

[0136] C2=(L2 / L)×100……………………(2)

[0137] C3=(L3 / L)×100……………………(3)

[0138] Where: C1—aromatic volume fraction, %;

[0139] C2—olefin volume fraction, %;

[0140] C3—volume fraction of saturated hydrocarbons, %;

[0141] L1—Aromatic region length, in millimeters (mm);

[0142] L2—olefin region length, in millimeters (mm);

[0143] L3—saturated hydrocarbon region length, in millimeters (mm);

[0144] L—the sum of L1+L2+L3, in millimeters (mm)

[0145] Table 2 Comparison of results of different modes

[0146]

[0147] Comparative Example 2

[0148] The operation in the comparative example was repeated. The hydrocarbon composition of the gasoline sample was measured using the hydrocarbon measuring device of the present invention.

[0149] 1. Test instruments and reagents

[0150] Instrument: The hydrocarbon determination device of the present invention.

[0151] Silica gel: Meet the following specifications: Surface area 430-530m 2 / g; pH value of 5% aqueous suspension is 5.5-7.0; 955℃ ignition loss (mass fraction): 4.5-10.0%; iron content (calculated as Fe2O3, dry basis): ≤50mg / kg.

[0152] Determination of pH value: Calibrate the pH meter with standard buffer solutions with pH values ​​of 4 and 7, place 5g of silica gel in a 250mL beaker, add 100mL of water and a stirring rod, stir on a magnetic stirrer for 20 minutes, and then use a calibrated pH meter to determine its pH value. Silica gel should be activated before use, placed in a shallow container, dried at 175°C for 3 hours, and placed in a sealed container while hot to prevent moisture.

[0153] Fluorescent indicator dyed silica gel: Standard dyed silica gel is obtained by recrystallizing Oil Red AB4 and olefin and aromatic dye purification parts obtained by chromatographic adsorption, and depositing them on silica gel through a specific procedure. Dyed silica gel should be stored in a dark place under normal pressure nitrogen, so that the dyed silica gel can have a service life of at least 5 years. It is best to take out a part of the dyed silica gel for daily use and put it in a small bottle to avoid affecting the service life of most of the dyed silica gel due to frequent use.

[0154] Isopropyl alcohol: analytical grade, content not less than 99%.

[0155] Compressed gas: air (or nitrogen), delivered to the top of the adsorption column at a controllable pressure range of 0kPa-103kPa.

[0156] Buffer solutions: pH values ​​are 4 and 7 respectively.

[0157] Mixed oil: intermediate product from a domestic petrochemical plant.

[0158] 2. Test steps

[0159] 1) Filling with silica gel

[0160] Place a small piece of absorbent cotton between the spherical ground mouth and the spherical socket at the end of the cleaned adsorption column, and clamp it with a small steel clamp. Turn on the vibrator and fill the silica gel while vibrating. When the separation section is half filled, stop vibrating, fill 3-5mm fluorescent indicator, then fill some silica gel, and then start vibrating again, so that the silica gel is filled to 75mm in the feeding section, and then stop vibrating after 4 minutes. Turn on the air purification device. Adjust the wind speed to 10m / s.

[0161] 2) Take samples

[0162] Use a sampler to extract 0.75±0.03ml of standard sample, insert the needle into the silica gel 30mm and inject the sample to allow the sample to be fully adsorbed.

[0163] 3) Inject reagent

[0164] After all the samples are adsorbed, inject isopropanol into the feeding section to the spherical joint, connect the top of the adsorption column to the air supply system, and clamp the spherical ground joint with a clamp.

[0165] 4) Pressurization

[0166] Maintain the pressure at 14kPa±2kPa for 2.5min±0.5min to allow the liquid to move downward along the adsorption column. Then increase the pressure to 34kPa±2kPa and maintain it for another 2.5min±0.5min, and finally adjust the air pressure to an appropriate pressure to allow the liquid to move downward.

[0167] 5) Start the temperature control device and adjust the temperature to 30°C.

[0168] 6) Reading

[0169] When the red alcohol-aromatic interface enters the analysis section about 350mm, quickly mark the interfaces of various hydrocarbons observed under ultraviolet light in the following order (from bottom to top) to measure a set of data. For the non-fluorescent saturated hydrocarbon area, mark the front edge of the sample and the position where the yellow fluorescence first reaches the strongest; for the second part, i.e., the upper end of the olefin area, mark the position where the strong blue fluorescence first appears; for the third part, i.e., the upper end of the aromatic area, mark the upper end of the first red or brown ring.

[0170] 3. Test results

[0171] After the above operation, the area lengths of the aromatic, olefin and saturated hydrocarbon bands are obtained, and the volume percentage of each hydrocarbon is calculated according to formula (1-3). The comparison of the results with and without heating is shown in Table 3.

[0172] C1=(L1 / L)×100……………………(1)

[0173] C2=(L2 / L)×100……………………(2)

[0174] C3=(L3 / L)×100……………………(3)

[0175] Where: C1—aromatic volume fraction, %;

[0176] C2—olefin volume fraction, %;

[0177] C3—volume fraction of saturated hydrocarbons, %;

[0178] L1—Aromatic region length, in millimeters (mm);

[0179] L2—olefin region length, in millimeters (mm);

[0180] L3—saturated hydrocarbon region length, in millimeters (mm);

[0181] L—the sum of L1+L2+L3, in millimeters (mm)

[0182] Table 3 Comparison of results of different modes

[0183]

[0184] The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content disclosed above to change or modify it into an equivalent embodiment with equivalent changes and apply it to other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A hydrocarbon determination device, characterized in that: include: A box body, and heating devices symmetrically fixed on both sides of the inner wall of the box body; A temperature control box is located on the upper right side of the box body, and the heating device is connected to the temperature control box through a signal control line; A temperature control probe is fixed in the box; An air purification device is located at the upper edge of the interior of the box, and the air purification device includes a first exhaust fan; a second exhaust fan is also provided at the upper edge of the interior of the box; A wind speed control box is arranged below the temperature control box, and the wind speed control box is connected to the first exhaust fan and the second exhaust fan; An analysis column and a ruler arranged parallel to the analysis column, wherein the reading module is nested on the ruler and slides on the ruler in a vertical direction.

2. The hydrocarbon measuring device according to claim 1, characterized in that: The heating devices located on the same side are distributed up and down.

3. The hydrocarbon measuring device according to claim 1, characterized in that: A first fixed thin rod and a second fixed thin rod are symmetrically fixed in the box body, the first fixed thin rod and the second fixed thin rod have upper and lower ends fixed on the box body, and the temperature control probe is fixed on the first fixed thin rod and the second fixed thin rod; There are two scales, namely a first scale and a second scale. The first scale is arranged in parallel on the left side of the first fixed thin rod, and the second scale is arranged in parallel on the right side of the second fixed thin rod.

4. The hydrocarbon measuring device according to claim 3, characterized in that: A first fixing rod and a second fixing rod are symmetrically arranged in the box body, both ends of the first fixing rod and the second fixing rod are fixed to the box body, a first fixing clamp and a first fixing knob are installed on the first fixing rod, and the first fixing knob is used to fix the first ultraviolet lamp, the first analytical column and the first ruler in sequence, and a first reading module is nested on the first ruler; A second fixing clamp and a second fixing knob are installed on the second fixing rod, and the second fixing knob is used to fix the second ultraviolet lamp, the second analysis column and the second ruler in sequence. The second reading module is nested on the second ruler, and the first analysis column and the second analysis column are respectively connected to gas pipelines.

5. The hydrocarbon measuring device according to claim 4, characterized in that: The number of the second row of fans is two, which are respectively located between the heating device and the first fixing rod, and between the heating device and the second fixing rod.

6. The hydrocarbon measuring device according to claim 3, characterized in that: The air purification device is arranged between the first fixed thin rod and the second fixed thin rod. The air purification device also includes an exhaust hood, an aluminum foil tube and an adsorption module which are connected in sequence. The adsorption module includes activated carbon filler, PP cotton filler and composite filler.

7. The hydrocarbon measuring device according to claim 1, characterized in that: The analytical column is made of a precision inner diameter glass tube or a standard wall glass tube, and comprises a feeding section with a capillary neck, a separation section and an analysis section; or is made of a standard wall glass tube.

8. The hydrocarbon measuring device according to claim 1, characterized in that: The hydrocarbon determination device also includes a control system, which implements operation program control through a control panel, and a pressure gauge, a power control switch and a pressure control switch are installed on the control panel.

9. The hydrocarbon measuring device according to claim 1, characterized in that: The first row of fans and the second row of fans can adjust the wind speed, which is divided into first gear, second gear and third gear.

10. A method for measuring hydrocarbon composition, using the hydrocarbon measuring device according to any one of claims 1 to 9, characterized in that: The hydrocarbon composition determination method comprises the following steps: Turn on the air purification device, adjust the wind speed control box, set the appropriate wind speed, fill the analytical column with filler and dyed silica gel, extract the sample and inject it into the analytical column, add organic reagent, connect the gas pipeline, pressurize the sample to separate in the analytical column, and turn off the air purification device; Turn on the exhaust fan, adjust the wind speed control box to set the appropriate wind speed, and adjust the temperature control box to set the temperature to a suitable temperature. At this time, the heating device starts heating. When the temperature control probe detects that the box temperature reaches the set temperature, the heating device automatically stops heating. Aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample move from top to bottom of the analytical column, and are repeatedly adsorbed and desorbed on the analytical column, so that the aromatic hydrocarbons, olefins and saturated hydrocarbons in the sample are separated in order of strength on the adsorption column. Fluorescent dyes are also selectively separated together with aromatic hydrocarbons, olefins and saturated hydrocarbons, so that the interface of aromatic hydrocarbons, olefins and saturated hydrocarbons produces red, blue, yellow and colorless spectrum bands under ultraviolet light. Turn on the UV lamp, and when the red interface enters the analysis section about 350 mm, move the reading module to calculate the volume percentage of each hydrocarbon based on the area length of the aromatic, olefin and saturated hydrocarbon bands in the analysis column.

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