CN103308469A - Device and method for automatically detecting acid value of petroleum product through reflux method - Google Patents

Device and method for automatically detecting acid value of petroleum product through reflux method Download PDF

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Publication number
CN103308469A
CN103308469A CN2013102501429A CN201310250142A CN103308469A CN 103308469 A CN103308469 A CN 103308469A CN 2013102501429 A CN2013102501429 A CN 2013102501429A CN 201310250142 A CN201310250142 A CN 201310250142A CN 103308469 A CN103308469 A CN 103308469A
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titration
cell
titration cell
cpu
syringe needle
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CN103308469B (en
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张庆乾
智洪彬
胡继刚
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Shandong Ketong Electric Technology Co. Ltd
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ZIBO KETONG ELECTRICAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a device and method for automatically detecting the acid value of a petroleum product through a reflux method, belonging to the technical field of analysis instruments of petroleum products. The device comprises a titration cell (7), a stirring device and a heating device arranged at the bottom of the titration cell (7), and a titration apparatus arranged above the titration cell and is characterized in that the bottom of the titration cell (7) extends outwards to form a liquid separation pool (21), photoelectric detection devices are fixed on two sides of the liquid separation pool, and a titration reflux interface is formed in the opening of the titration cell (7). The method comprises the following detection steps that: the device enters a working state and initializes to set functions, the device begins the detection work, an operator selects whether to clean the device before shut down or perform the next test after the detection, and the device performs the next operation according to the selection of the operator. The reflux method is adopted by the device and method disclosed by the invention, steps, such as cleaning, liquid adding, heating, stirring, measuring and metering are automatically finished in the same titration cell, and the detection precision is higher.

Description

Utilize petroleum products acid number automatic detection device and the detection method of circumfluence method
Technical field
Utilize petroleum products acid number automatic detection device and the detection method of circumfluence method, belong to the petroleum product analysis Instrument technology field.Be specifically related to a kind of employing circumfluence method the petroleum products acid number is detected, can finish petroleum products acid number automatic detection device and the detection method of functions such as auto injection, automatic liquid feeding, automatic gauge, measurement automatically, cleaning automatically, automatic drain.
Background technology
The petroleum products acid number is an important indicator that detects the check petroleum products.When the acidity of carrying out petroleum products detects, at first with the extract of a certain amount of product to be detected and corresponding proportion, heat then, add indicator after the boiling, and splash into neutralizing agent when liquid constantly stirred, when the neutralizing agent that adds two with in the acid number of detected sample is lucky and the time, the indicator color is undergone mutation, stop to add neutralizing agent this moment, calculates the acid number of product to be detected then by the amount of calculating added neutralizing agent.
In the prior art, petroleum products is carried out mainly adopting two kinds of methods when acid number detects: (1) is manually detected, and the defective of the method is that work is loaded down with trivial details, and workload is big and error is bigger; (2) detect automatically by automatic tester, the color for the treatment of tracer liquid by the light sensation device detects.But when using automatic testing method, if it is less to hold the vessel radius of liquid to be detected, then inconvenience stirs liquid, irregular phenomenon can occur stirring; If the radius of container is bigger, then present light sensation technology is difficult to pass thicker container and detects.At present the way that generally adopts is after product to be detected and extract are fully mixed boiling, be drawn into and carry out in the titration in the less container of another one radius and test, but when being to use this method, in the process that extracts, the one, the loss of temperature can appear, when particularly room temperature is lower, the 2nd, the tube wall that extracts can stay certain liquid, bigger measuring error can occur equally.So, in short supply current technician, under the big situation of labor intensive, invent a kind of can realize the automatic liquid feeding of petroleum products acid value measuring instrument, measurement automatically, automatic gauge, automatically a series of processes such as cleaning robotization and accurately detect product acid number product to be measured and become particularly important.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provide a kind of circumfluence method that adopts can finish higher petroleum products acid number automatic detection device and the detection method of utilizing circumfluence method of high precision detection automatically in same titration cell.
The technical solution adopted for the present invention to solve the technical problems is: this utilizes the petroleum products acid number automatic detection device of circumfluence method, the titration cell that comprises cup-shaped, be arranged on stirring apparatus and the heating arrangement of titration cell bottom, and the titration apparatus that is arranged on the titration cell top, it is characterized in that: described titration cell bottom one epitaxial lateral overgrowth is stretched and is formed a separating pool, the both sides of separating pool are fixing by the photoelectric detection system of being made up of photoemission cell and photoelectric receiving tube, and the titration cell oral area is provided with the titration backflow interface that is connected with titration cell inside.
Described separating pool is that diameter is 15 ~ 25mm, the cylindrical structural of cutting edge in the left and right sides.
Described titration backflow interface comprises buret and the condenser pipe lower fixed hole that protrudes from titration cell oral area upper surface, the upper coarse and lower fine right side that is arranged at the titration cell oral area of condenser pipe lower fixed hole, buret is arranged on the left side of condenser pipe lower fixed hole, the left side of condenser pipe lower fixed hole is disposed with the temperature sensor lower fixed hole that communicates with titration cell inside simultaneously and adds the discharging tube lower fixed hole, and described titration apparatus matches with buret and the condenser pipe lower fixed hole of titration cell oral area.
Described buret is that two front and back are symmetrical arranged.
Described titration apparatus comprises and is fixed on two titration syringe needles and two grooved photoelectricity couplings that titration covers, two grooved photoelectricity couplings are fixed in the photoelectricity coupling pickup groove of titration lid bottom and are corresponding with two burets respectively, and the titration syringe needle passes the titration lid from top to bottom and the corresponding titration syringe needle jack that is arranged on grooved photoelectricity coupling center that inserts is placed in the corresponding buret;
The upper surface of titration lid is disposed with fixed orifice on the condenser pipe from back to front, fixed orifice and add fixed orifice on the discharging tube on the temperature sensor, on the temperature sensor on fixed orifice and the condenser pipe between the fixed orifice level and left-right symmetric respectively be provided with a titration syringe needle fixed orifice and at the lead fairlead of titration syringe needle fixed orifice both sides, the front end of each titration syringe needle fixed orifice is provided with a titration syringe needle pickup groove that communicates with it;
Fixed orifice and add fixed orifice on the discharging tube respectively with condenser pipe lower fixed hole, the temperature sensor lower fixed hole of titration cell oral area with add the discharging tube lower fixed hole and be connected on fixed orifice, the temperature sensor on the described condenser pipe; Each titration syringe needle fixed orifice is connected with the center of a photoelectricity coupling pickup groove respectively.
Described stirring apparatus is magnetic stirring apparatus, comprises the magnetic stir bar that is placed on titration cell inside and the magnetic agitation motor that is fixed on the titration cell below.
Described heating arrangement comprises electrothermal tube and well heater, well heater is for respectively being provided with the sheet metal of a groove up and down, the intersection of the two grooves formation fixed station that stretches out up and down, be placed on the pedestal by thermal sleeve around the fixed station, and by bolt, electrothermal tube places in the groove border of heater base.
Described heating arrangement comprises electrothermal tube and well heater, well heater is for respectively being provided with the sheet metal of a groove up and down, the intersection of the two grooves formation fixed station that stretches out up and down, be placed on the pedestal by thermal sleeve around the fixed station, and by bolt, electrothermal tube places in the groove border of heater base.
Utilize the petroleum products acid number automatic testing method of circumfluence method, it is characterized in that: use the petroleum products acid number automatic detection device of above-mentioned circumfluence method to detect, step is as follows:
Step 1001, beginning, after the electric power starting, this automatic detection device enters duty;
Step 1002 is installed initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to the function setting flow process, and after setting was finished, this automatic detection device carried out work according to setting;
Step 1004, the cleaning before judging whether to shut down is after the work of this automatic detection device is finished, cleaning before whether display prompts shuts down, if can shut down and clean this moment, then select "Yes" by button, then execution in step 1005; If do not need to clean, then select "No" by button, then execution in step 1006; Carry out next one test if desired, select " cancellation " by button, return step 1003;
Step 1005 is cleaned, and CPU control is cleaned titration cell and internal pipeline;
Step 1006, shutdown, the work of this automatic detection device finishes, automatically shutdown.
Function setting flow process described in the step 1003 the steps include:
Step 2001, the interface initialization, the display interface of CPU carries out initialization;
Step 2002, CPU has judged whether button input, CPU is, and button scans, and whether the decision operation personnel carried out the instruction input by button, if there is not the button input, then proceeds key scan; If operating personnel have selected " instrument self checking " function by button, then execution in step 2003; As selected " test " function, and then execution in step 2004, if selected " parameter setting " function, then execution in step 2005, if selected " shutdown " then execution in step 2006;
Step 2003, instrument self checking, CPU carries out status detection to execution unit in this automatic detection device;
Step 2004 is tested, and CPU controls this automatic detection device and tests according to the process of the test flow process;
Step 2005, parameter is set, and operating personnel carry out the setting of test parameters again;
Step 2006, shutdown, power-off operation is carried out in CPU control.
Process of the test flow process described in the step 2002 the steps include:
Step 3001 is cleaned for the first time, and CPU control peristaltic pump pumps alcohol cleans titration cell inside and internal duct, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump was discharged equally;
Step 3002 is measured test products, and the product to be measured of CPU control peristaltic pump pumps 10mL enters in the buret;
Step 3003, the unnecessary product to be measured of emptying, CPU control peristaltic pump is discharged product to be measured unnecessary in the pipeline;
Step 3004 is cleaned for the second time, and CPU control peristaltic pump pumps alcohol carries out the cleaning second time to titration cell inside and internal duct, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump was discharged equally;
Step 3005 is injected product to be measured and extract, and CPU control peristaltic pump injects the product to be measured of the 10mL in the buret in the titration cell, measures the extract of 50mL then equally by buret, injects in the titration cell equally;
Step 3006, heating, condensation, CPU controls electrothermal tube work, and by well heater titration cell is heated, and in the process of heating, extract constantly evaporates, and evaporation passes back into again in the titration cell after entering condenser pipe, so circulation;
Step 3007, CPU judges whether product to be measured in the titration cell and the mixed liquor of extract seethe with excitement, if seethe with excitement, then execution in step 3008, if step 3006 is returned in also not boiling;
Step 3008 begins to stir, and the work of CPU control magnetic stirring apparatus is stirred the mixed liquor in the titration cell, and mixing time is 5min;
Step 3009 is injected indicator, and the titration syringe needle dropwise splashes into indicator in titration cell, and the grooved photoelectricity symplectic quantity that splashes into corresponding with this titration syringe needle detected and calculated by CPU this moment, reaches dosage and stops to splash into of indicator afterwards;
Step 3010, beginning titration, Photoelectric Detection also calculated, in titration cell, dropwise splash into neutralizing agent by another titration syringe needle, at this moment, the grooved photoelectricity symplectic quantity that splashes into corresponding with this titration syringe needle detects and concrete quantity is sent to CPU, and calculates by display screen by CPU and to show; The photoelectric detection system of CPU control is simultaneously started working, and detects the variation of liquid color in the separating pool;
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point then execution in step 3012, if the no show titration end-point is returned step 3010;
Step 3012 stops heating, titration, Photoelectric Detection and calculates, and the titration syringe needle that CPU control splashes into neutralizing agent stops to splash into neutralizing agent, and stop to continue heating simultaneously and stir, and the final acid number of the data computation product to be measured by the transmission of grooved photoelectricity coupling;
Step 3013, CPU judges whether and need print net result, prints if desired, execution in step 3014 is not if need to print execution in step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015 finishes, and process of the test finishes.
Compared with prior art, the beneficial effect that has of the present invention is:
1, can in same titration cell, finish steps such as cleaning, liquid feeding, heating, stirring, measurement and metering automatically by automatic detection device of the present invention, after having solved prior art product to be detected and extract fully being mixed boiling, need be drawn into and carry out in the titration in the less container of another one radius and test, because temperature descends and to cause temperature inaccurate, and the tube wall that extracts can stay certain liquid and causes the bigger problem of measuring error thus in the extraction process.Really realized the high precision detection.
2, separating pool is that diameter is 15 ~ 25mm, the cylindrical structural of cutting edge in the left and right sides, thus make light can better pass the interior liquid of separating pool, make detection more accurate.
3, designed and the matching used titration lid of titration cell, adopted the amount of splashing into of the symplectic neutralizing agent of grooved photoelectricity and indicator to calculate, it is more accurate to make that product acid number to be detected calculates.
4, according to the characteristic of indicator, adopted the photoemission cell that sends blue light, make more light can pass the interior liquid of separating pool.
5, adopted circumfluence method, thereby in heating process, the extract that evaporates is back in the titration cell again, thereby has avoided the consumption of the extract that causes because of heating, make result calculated more accurate.
6, adopt the design of condenser pipe, can reduce the drain evaporation of extract in the titration cell to the full extent.
7, adopted single-chip microcomputer to control as the duty of the complete machine of CPU, duty is more reliable.
8, the light that sends of photoemission cell is blue light, with finish just in and the time indicator color identical, thereby can make the easier intensity variations that detects of photoelectric receiving tube.
9, simple in structure, and the parts that adopt are universal component, reliability is high and be easy to change.
Description of drawings
Fig. 1 is the petroleum products acid number automatic detection device structural representation that utilizes circumfluence method.
Fig. 2 is the vertical view of Fig. 1.
Fig. 3 is the petroleum products acid number automatic detection device titration cell front view that utilizes circumfluence method.
Fig. 4 is the petroleum products acid number automatic detection device titration cell right view that utilizes circumfluence method.
Fig. 5 is the petroleum products acid number automatic detection device titration cell vertical view that utilizes circumfluence method.
Fig. 6 utilizes the petroleum products acid number automatic detection device titration of circumfluence method to cover main pseudosection.
Fig. 7 is the petroleum products acid number automatic detection device titration lid vertical view that utilizes circumfluence method.
Fig. 8 utilizes the petroleum products acid number automatic testing method of circumfluence method to detect flow chart of steps.
Fig. 9 is the petroleum products acid number automatic testing method function setting process flow diagram that utilizes circumfluence method.
Figure 10 is the petroleum products acid number automatic testing method process of the test process flow diagram that utilizes circumfluence method.
Wherein: 1, temperature sensor 2, photoelectricity coupling lead 3, titration syringe needle 4, titration lid 5, holding screw 6, grooved photoelectricity coupling 7, titration cell 8, magnetic stir bar 9, magnetic force rotary head 10, electrothermal tube 11, well heater 12, magnetic agitation motor 13, thermal sleeve 14, pedestal 15, seal gasket 16, add discharging tube 17, peristaltic pump 18, photoemission cell 19, photoelectric receiving tube 20, backboard 21, separating pool 22, buret 23, condenser pipe lower fixed hole 24, temperature sensor lower fixed hole 25, add discharging tube lower fixed hole 26, fixed orifice 27 on the temperature sensor, lead fairlead 28, screw hole 29, titration syringe needle fixed orifice 30, photoelectricity coupling pickup groove 31, fixed orifice 32 on the condenser pipe, titration syringe needle pickup groove 33, add fixed orifice on the discharging tube.
Embodiment
Fig. 1 ~ 10th, most preferred embodiment of the present invention, the present invention will be further described below in conjunction with accompanying drawing 1 ~ 10.
Shown in Fig. 1 ~ 2, the petroleum products acid number automatic detection device (to call automatic detection device in the following text) of circumfluence method that utilizes of the present invention mainly is made up of following components: the titration apparatus that titration cell 7 and cooperate with titration cell 7 is installed, photoelectric detection system, stirring apparatus, heating arrangement, condenser pipe carried out backflow refrigerating plant and the input-output unit of refrigeration.Wherein input-output unit comprises the button of realizing that function is selected, the display that duty is shown and the printing equipment that net result is printed.The duty of whole detection device is controlled by control circuit, and it is that the single-chip microcomputer of STM32F1032ET carries out the realization of function as CPU that control circuit has adopted model.
Heating arrangement comprises electrothermal tube 10 and well heater 11.Well heater 11 is the rectangular metal device, and its top and bottom respectively are provided with the groove of a circle, and titration cell 7 is placed in the groove at its top.Be protruding with fixed station at the intersection of two grooves up and down, the fixed station below is placed with thermal sleeve 13, after thermal sleeve 13 installations, by screw bolt passes fixed station and thermal sleeve 13, well heater 11 is fixed to pedestal 14 tops, after fixedly finishing, the groove of well heater 11 bottoms is embedded in the pedestal 14.Electrothermal tube 10 is positioned at the groove border of well heater 11 bottoms.
Stirring apparatus comprises the magnetic stirring apparatus that is positioned at well heater 11 belows, and magnetic agitation motor 12 tops in the magnetic stirring apparatus link to each other with magnetic force rotary head 9 bottoms, and the top of magnetic force rotary head 9 places in the groove of well heater 11 bottoms.The magnetic stir bar of using 8 that matches with magnetic force rotary head 9 is positioned over titration cell 7 inside.
Titration apparatus comprise with titration cell 7 be used be installed on the titration lid 4 two titration syringe needles 3 and with two grooved photoelectricity couplings 6 that match respectively at each titration syringe needle 3.
Titration lid 4 is rectangular block shape, is placed on titration cell 7 tops, and its bottom centre position both sides respectively are provided with a groove, and a grooved photoelectricity coupling 6 is fixedly arranged in each groove, is placed with a seal gasket 15 between each grooved photoelectricity coupling 6 and the titration lid 4.Two photoelectricity coupling leads 2 that link to each other with grooved photoelectricity coupling 6 cover 4 upper surfaces from titration draws.Each grooved photoelectricity coupling 6 equal correspondence is provided with a titration syringe needle 3, two titration syringe needles 3 pass titration lid 4 from top to bottom, the bottom of each titration syringe needle 3 is positioned at corresponding grooved photoelectricity coupling 6 centers, grooved photoelectricity coupling 6 quantity for detection of the liquid that oozes from titration syringe needle 3.After titration lid 4 covered above titration cell 7, two burets 22 on the titration cell 7 were stuck in the grooved mouth of a grooved photoelectricity coupling 6, and the syringe needle of titration simultaneously 3 enters the inside of corresponding buret 22.
Temperature sensor 1 and add discharging tube 16 and pass the bottom that titration lid 4 and titration cell 7 are placed on titration cell 7 simultaneously from top to bottom successively adds peristaltic pump 17 is installed on the discharging tube 16.
Photoelectric detection system comprises photoemission cell 18 and photoelectric receiving tube 19, photoemission cell 18 and photoelectric receiving tube 19 simultaneously by bolt on the backboard 20 at its back side.Extending from titration cell 7 bottom rear has separating pool 21, and separating pool 21 is between photoemission cell 18 and photoelectric receiving tube 19, so that the change color that photoemission cell 18 and photoelectric receiving tube 19 detect in the separating pools 21.
Temperature sensor 1, photoemission cell 18 and photoelectric receiving tube 19 link to each other with CPU simultaneously.
Shown in Fig. 3 ~ 5, titration cell 7 is glass cup-like containers processed, and portion treats testing product and stirs titration operation within it.The bottom rear of titration cell 7 is parallel to stretch out and is provided with separating pool 21, and separating pool 21 is for cylindrical and communicate with titration cell 7 inside.Separating pool 21 is 15 ~ 25mm for diameter, the cylindrical structural of cutting edge in the left and right sides.Being convenient to photoelectric detection system detects the liquid in it.
The oral area of titration cell 7 has condenser pipe lower fixed hole 23 for partly sealing design on its oral area right side, and condenser pipe lower fixed hole 23 left sides are disposed with temperature sensor lower fixed hole 24 and add discharging tube lower fixed hole 25.Temperature sensor lower fixed hole 24 is provided with two burets 22 with the symmetria bilateralis that adds discharging tube lower fixed hole 25, and buret 22 protrudes from the upper surface of titration cell 7 oral areas.Buret 22, condenser pipe lower fixed hole 23, temperature sensor lower fixed hole 24 and add discharging tube lower fixed hole 25 and be all the through hole that communicates with titration cell 7 inside, and the part that buret 22 and condenser pipe lower fixed hole 23 are in titration cell 7 oral areas is upper coarse and lower fine conical design, and buret 22 is last inferior thick design above the part of titration cell 7 oral areas.
Shown in Fig. 6 ~ 7, titration lid 4 is for cuboid designs, and the two bottom sides symmetry of titration lid 4 respectively is provided with the photoelectricity coupling pickup groove 30 of a rectangle.Each photoelectricity coupling pickup groove 30 left and right sides edge respectively is provided with a screw hole 28.
The upper surface rear portion of titration lid 4 is provided with fixed orifice 31 on the condenser pipe, fixed orifice 31 the place aheads are disposed with on the temperature sensor fixed orifice 26 and add fixed orifice 33 on the discharging tube on the condenser pipe, fixed orifice 26 and add that fixed orifice 33 each side is symmetrically arranged with a titration syringe needle fixed orifice 29 on the discharging tube on the temperature sensor, each titration syringe needle fixed orifice 29 each side is symmetrically arranged with a lead fairlead 27, and the front end of each titration syringe needle fixed orifice 29 is provided with one and extends to the titration syringe needle pickup groove 32 that 4 front ends are covered in titration.Each group titration syringe needle fixed orifice 29 with and lead fairlead 27 correspondences of both sides and be positioned at the photoelectricity coupling pickup groove 30 that 4 bottoms are covered in titration, and each titration syringe needle fixed orifice 29 all is positioned at the center of corresponding photoelectricity coupling pickup groove 30.Temperature sensor lower fixed hole 24 and add on the discharging tube fixed orifice 33 side by side about between two photoelectricity coupling pickup grooves 30.
Fixed orifice 26 and add fixed orifice 33 on the discharging tube and be the through hole of UNICOM up and down on fixed orifice 31, lead fairlead 27, the temperature sensor on above-mentioned titration syringe needle fixed orifice 29, the condenser pipe.Wherein fixed orifice 31 is upper coarse and lower fine conical through-hole on the condenser pipe; Two titration syringe needle fixed orifices 29 are the through hole of upper coarse and lower fine step cutting pattern shape.Fixed orifice 26 is similarly the through hole of upper coarse and lower fine step cutting pattern shape on the temperature sensor.
Shown in Fig. 6 ~ 7, two grooved photoelectricity couplings 6 are placed on titration respectively and cover in the photoelectricity coupling pickup groove 30 of 4 bottoms, be provided with a seal gasket 15 between the grooved photoelectricity coupling 6 of each side and the titration lid 4, and by both sides totally four holding screws 5 screw in corresponding screw holes 28, the seal gasket 15 of two grooved photoelectricity couplings 6 and top is fixed in the photoelectricity coupling pickup groove 30 of respective side.All be connected with two photoelectricity coupling leads 2 on the grooved photoelectricity coupling 6 of each side, two photoelectricity coupling leads 2 of each side upwards pass seal gasket 15 and lead fairlead 27 successively and cover 4 tops from titration and draw.All be placed with a titration syringe needle 3 from top to bottom in the titration syringe needle fixed orifice 29 of each side.6 two of grooved photoelectricity couplings link to each other with CPU by corresponding photoelectricity coupling lead 2 respectively.
In the present invention, what titration syringe needle 3 adopted is the common transfusion bottle syringe needle that matches with transfusion bottle, and such transfusion bottle syringe needle comprises the plastics end of upper end and the thinner metal needle of drawing from the plastics end, and plastics end one side is provided with a plastic handles.This titration syringe needle 3 is passed titration syringe needle fixed orifice 29 from top to bottom, the plastics section that titration syringe needle 3 upper ends are thicker and the thinner metal needle of drawing from the plastics end and the titration syringe needle fixed orifice 29 upper coarse and lower fine designs installation that matches, and the plastic handles of titration syringe needle 3 tops is stuck in the corresponding titration syringe needle pickup groove 32, and titration syringe needle 3 is fixing.The fluid place, bottom of titration syringe needle 3 all was in the center of corresponding grooved photoelectricity coupling 6 after the titration syringe needle 3 of each side was fixedly finished.
After titration apparatus is fixedly finished, can the corresponding top of covering titration cell 7.At this moment, two outstanding on the titration cell 7 burets 22 are corresponding with a grooved photoelectricity coupling 6 respectively, and snap between the corresponding grooved photoelectricity coupling 6, the bottom of the titration syringe needle 3 that is positioned at grooved photoelectricity coupling 6 centers of each side all enters corresponding buret 22 inside.Be arranged at simultaneously on the titration lid 4 add on the discharging tube fixed orifice 26 on fixed orifice 31 on fixed orifice 33, the condenser pipe and the temperature sensor respectively be arranged on titration cell 7 oral areas to add discharging tube lower fixed hole 25, condenser pipe lower fixed hole 23 and temperature sensor lower fixed hole 24 corresponding, and adding discharging tube 16 passes successively and adds on the discharging tube fixed orifice 33 and add discharging tube lower fixed hole 25, temperature sensor 1 passes fixed orifice 26 on the temperature sensor successively, temperature sensor lower fixed hole 24 stretches in the titration cell 7, is positioned at the bottom of titration cell 7.Condenser pipe passes successively on the condenser pipe that its lower end is positioned at titration cell 7 after the fixed orifice 31 and condenser pipe lower fixed hole 23.
After the condenser pipe installation, the backflow refrigerating plant in the automatic detection device of the present invention is connected with the cold-producing medium circulation mouth of pipe that is arranged on the condenser pipe above and below respectively, and condensing agent circulates within it.Condenser pipe carries out condensation to the extract that is evaporated in the condenser pipe, and vaporous extract condenses into liquid and is back in the titration cell 7 at the inwall of condenser pipe through the condensation of condenser pipe, remains unchanged with the dosage that guarantees extract.The backflow refrigerating plant is ripe prior art, can realize that also can pass through compressed refrigerant, the mode of freezing by cold-producing medium realizes by water circulation way.
In automatic detection device of the present invention, after the product to be measured in the titration cell 7 is finished neutralization, can the acid number of product to be measured be calculated, and print by printing device.
Be illustrated in figure 8 as the petroleum products acid number automatic testing method of circumfluence method that utilizes of the present invention and detect flow chart of steps, its concrete steps are:
Step 1001, beginning, after the electric power starting, this automatic detection device enters duty;
Step 1002 is installed initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to the function setting flow process, and after setting was finished, this automatic detection device carried out work according to setting;
Step 1004, the cleaning before judging whether to shut down is after the work of this automatic detection device is finished, cleaning before whether display prompts shuts down, if can shut down and clean this moment, then select "Yes" by button, then execution in step 1005; If do not need to clean, then select "No" by button, then execution in step 1006; Carry out next one test if desired, select " cancellation " by button, return step 1003;
Step 1005 is cleaned, and CPU control is cleaned titration cell and internal pipeline;
Step 1006, shutdown, the work of this automatic detection device finishes, automatically shutdown.
Be illustrated in figure 9 as the petroleum products acid number automatic testing method function setting process flow diagram that utilizes circumfluence method of the present invention, its concrete steps are:
Step 2001, the interface initialization, the display interface of CPU carries out initialization;
Step 2002, CPU has judged whether button input, CPU is, and button scans, and whether the decision operation personnel carried out the instruction input by button, if there is not the button input, then proceeds key scan; If operating personnel have selected " instrument self checking " function by button, then execution in step 2003; As selected " test " function, and then execution in step 2004, if selected " parameter setting " function, then execution in step 2005, if selected " shutdown " then execution in step 2006;
Step 2003, instrument self checking, CPU carries out status detection to execution unit in this automatic detection device;
Step 2004 is tested, and CPU controls this automatic detection device and tests according to the process of the test flow process;
Step 2005, parameter is set, and operating personnel carry out the setting of test parameters again;
Step 2006, shutdown, power-off operation is carried out in CPU control.
The state-detection of execution unit mainly comprises the situation of closing of solenoid valve in the pipeline and the running status of pump.
Be the petroleum products acid number automatic testing method process of the test process flow diagram that utilizes circumfluence method of the present invention as shown in figure 10, its concrete steps are:
Step 3001 is cleaned for the first time, and CPU control peristaltic pump 17 extracts alcohol titration cell 7 inside and internal duct are cleaned, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump 17 was discharged equally;
Step 3002 is measured test products, and the product to be measured that CPU control peristaltic pump 17 extracts 10mL enters in the buret;
Step 3003, the unnecessary product to be measured of emptying, CPU control peristaltic pump 17 is discharged product to be measured unnecessary in the pipeline;
Step 3004, clean the second time, and CPU control peristaltic pump 17 extracts alcohol the cleaning second time is carried out in titration cell 7 inside and internal duct, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump 17 was discharged equally;
Step 3005 is injected product to be measured and extract, and CPU control peristaltic pump 17 injects the product to be measured of the 10mL in the buret in the titration cell 7, measures the extract of 50mL then equally by buret, injects equally in the titration cell 7;
Step 3006, heating, condensation, CPU control electrothermal tube 10 is worked, and heats by 11 pairs of titration cells 7 of well heater, and in the process of heating, extract constantly evaporates, and evaporation refluxes as in the titration cell 7 again after entering condenser pipe, so circulates;
Step 3007, CPU judges whether product to be measured in the titration cell 7 and the mixed liquor of extract seethe with excitement, if seethe with excitement, then execution in step 3008, if step 3006 is returned in also not boiling;
Step 3008 begins to stir, and the work of CPU control magnetic stirring apparatus is stirred the mixed liquor in the titration cell 7, and mixing time is 5min;
Step 3009 is injected indicator, and titration syringe needle 3 dropwise splashes into indicator in titration cell 7, and this moment and this titration syringe needle 3 corresponding 6 pairs of quantity that splash into of grooved photoelectricity coupling detect and calculate by CPU, stops to splash into of indicator after reaching dosage;
Step 3010, beginning titration, Photoelectric Detection also calculated, in titration cell 7, dropwise splash into neutralizing agent by another titration syringe needle 3, at this moment, grooved photoelectricity coupling 6 pair quantity of splashing into corresponding with this titration syringe needle 3 detect and concrete quantity are sent to CPU, and calculate by display screen by CPU and to show; The photoelectric detection system of CPU control is simultaneously started working, and detects the variation of liquid color in the separating pool 21;
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point then execution in step 3012, if the no show titration end-point is returned step 3010;
Step 3012, stop heating, titration, Photoelectric Detection and calculate, the titration syringe needle 3 that CPU control splashes into neutralizing agent stops to splash into neutralizing agent, stops to continue heating and stirring simultaneously, and passes through the final acid number of the data computation product to be measured of grooved photoelectricity coupling 6 transmission;
Step 3013, CPU judges whether and need print net result, prints if desired, execution in step 3014 is not if need to print execution in step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015 finishes, and process of the test finishes.
In this process of the test, adopt alcohol as extract.After beginning to heat, temperature sensor 1 carries out temperature detection, and real time temperature is passed to CPU, and CPU is, and temperature is calculated, and when calculating temperature when no longer significant change taking place, represents that then the mixed liquors in the titration cell 7 have reached fluidized state.
The concrete course of work is as follows: after the start of this automatic detection device, at first automatically, carry out the initialization of carrying out of cpu clock and peripheral apparatus, operating personnel carry out function setting then, if selected " instrument self checking " or " parameter setting " function, then this automatic detection device carries out corresponding function automatically, if selected " test " function, then carry out the test of product to be measured.
At first this automatic detection device injects alcohol by peristaltic pump 17 in pipeline and titration cell 7, carries out the flushing first time, and flushing is discharged waste alcohol after finishing automatically.By peristaltic pump 17 product to be measured is pumped in the buret that dosage is 10mL then, then unnecessary product to be measured is discharged, and carry out the second time and clean.Under the effect of peristaltic pump 17, through adding discharging tube 16 product to be measured of the 10mL in the buret is injected in the titration cell 7 then, divide the extract alcohol of measuring common 50mL for five times by buret equally then, inject in the titration cell 7 through adding discharging tube 16.
11 pairs of titration cells 7 of CPU control heater this moment heat.This moment, temperature sensor 1 began to detect the temperature of liquid in the titration cell 7, and detected temperature value is sent to CPU, that CPU when detecting mixed liquors in the titration cell 7 and being in fluidized state, CPU control magnetic stirring apparatus stirs the mixed liquor in the titration cell 7, and mixing time is 5 minutes.In titration cell 7, splash into a certain amount of indicator by a titration syringe needle 3 then, in the indicator titration process, the amount of the grooved photoelectricity coupling 6 pair indicator that splash into corresponding with this titration syringe needle 3 detects, when indicator splash into finish after, stop to splash into of indicator, and begin in titration cell 7, to splash into neutralizing agent by another titration syringe needle 3.
In the process that neutralizing agent splashes into, dripping of the neutralizing agent that grooved photoelectricity coupling 6 real time record of respective side splash into counted, and the photoemission cell 18 that is positioned at separating pool 21 1 sides simultaneously is luminous, and corresponding photoelectric receiving tube 19 receives the light that photoemission cells 18 send.When the acid number of amount that neutralizing agent adds and product to be detected just in and the time, the color change of the indicator in it, this moment, the light intensity of the light that photoelectric receiving tube 19 receives changed, and controlled titration syringe needle 3 and stopped to continue to splash into neutralizing agent.Well heater 11 and magnetic stirring apparatus quit work simultaneously.In the whole neutralization reaction process, CPU calculates the quantity of the neutralizing agent that splashes in real time, and shows at display.
The amount of last CPU by the neutralizing agent that splashed into calculates the acid number in the product to be detected.In entire test, extract constantly evaporates and enters and is arranged on titration and covers in the condenser pipe of 4 tops, and in condenser pipe cooling back was refluxed as titration cell 7, the amount of assurance titration cell 7 interior extracts remained unchanged.
After test was finished, whether operating personnel can select test findings to be printed, the cleaning before whether this automatic detection device judges whether to shut down and shut down then, and after above step was finished, this test finished.
In the present embodiment, what liquid carried out thermometric temperature sensor 1 employing in the titration cell 7 is the Pt1000 thermal resistance, also can adopt other sensors, as the temperature transmitter of Pt100 thermal resistance or outputting standard current signal.
What indicator adopted is the BTB indicator.Because during neutralizing agent is just finished with product to be detected and the time, the color change of this indicator is blue, so the light that photoemission cell 18 sends is for blue, can see through stronger light when indicator becomes blueness, what photoelectric receiving tube 19 adopted is commercially available common phototriode.
What condenser pipe adopted is common spherical condensation tube, can carry out condensation by condensate water or other cold-producing mediums in it.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment does, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.

Claims (10)

1. utilize the petroleum products acid number automatic detection device of circumfluence method, the titration cell (7) that comprises cup-shaped, be arranged on stirring apparatus and the heating arrangement of titration cell (7) bottom, and the titration apparatus that is arranged on titration cell (7) top, it is characterized in that: described titration cell (7) bottom one epitaxial lateral overgrowth is stretched and is formed a separating pool (21), fixedly there is the photoelectric detection system of being made up of photoemission cell (18) and photoelectric receiving tube (19) both sides of separating pool (21), and titration cell (7) oral area is provided with the titration backflow interface that is connected with titration cell (7) inside.
2. the petroleum products acid number automatic detection device that utilizes circumfluence method according to claim 1, it is characterized in that: described separating pool (21) is 15 ~ 25mm for diameter, the cylindrical structural of cutting edge in the left and right sides.
3. the petroleum products acid number automatic detection device that utilizes circumfluence method according to claim 1, it is characterized in that: described titration backflow interface comprises buret (22) and the condenser pipe lower fixed hole (23) that protrudes from titration cell (7) oral area upper surface, the upper coarse and lower fine right side that is arranged at titration cell (7) oral area of condenser pipe lower fixed hole (23), buret (22) is arranged on the left side of condenser pipe lower fixed hole (23), the left side of condenser pipe lower fixed hole (23) is disposed with the temperature sensor lower fixed hole (24) that communicates with titration cell (7) inside simultaneously and adds discharging tube lower fixed hole (25), and described titration apparatus matches with buret (22) and the condenser pipe lower fixed hole (23) of titration cell (7) oral area.
4. the petroleum products acid number automatic detection device that utilizes circumfluence method according to claim 3, it is characterized in that: described buret (22) is that two front and back are symmetrical arranged.
5. according to claim 1 or the 3 described petroleum products acid number automatic detection devices that utilize circumfluence method, it is characterized in that: described titration apparatus comprises two titration syringe needles (3) and two the grooved photoelectricity couplings (6) that are fixed on the titration lid (4), two grooved photoelectricity couplings (6) are fixed in the photoelectricity coupling pickup groove (30) of titration lid (4) bottom and are corresponding with two burets (22) respectively, and titration syringe needle (3) passes titration lid (4) from top to bottom and the corresponding titration syringe needle jack that is arranged on grooved photoelectricity coupling (6) center that inserts is placed in the corresponding buret (22);
The upper surface of titration lid (4) is disposed with fixed orifice on the condenser pipe (31) from back to front, fixed orifice on the temperature sensor (26) and add fixed orifice on the discharging tube (33), on fixed orifice on the temperature sensor (26) and the condenser pipe between the fixed orifice (31) level and left-right symmetric respectively be provided with a titration syringe needle fixed orifice (29) and at the lead fairlead (27) of titration syringe needle fixed orifice (29) both sides, the front end of each titration syringe needle fixed orifice (29) is provided with a titration syringe needle pickup groove (32) that communicates with it;
Fixed orifice (26) and add fixed orifice on the discharging tube (33) respectively with condenser pipe lower fixed hole (23), the temperature sensor lower fixed hole (24) of titration cell (7) oral area with add discharging tube lower fixed hole (25) and be connected on fixed orifice on the described condenser pipe (31), the temperature sensor; Each titration syringe needle fixed orifice (29) is connected with the center of a photoelectricity coupling pickup groove (30) respectively.
6. according to the petroleum products acid number automatic detection device that utilizes circumfluence method of claim 1, it is characterized in that: described stirring apparatus is magnetic stirring apparatus, comprises the magnetic agitation motor (12) that is placed on the inner magnetic stir bar (8) of titration cell (7) and is fixed on titration cell (7) below.
7. the petroleum products acid number automatic detection device that utilizes circumfluence method according to claim 1, it is characterized in that: described heating arrangement comprises electrothermal tube (10) and well heater (11), well heater (11) is for respectively being provided with the sheet metal of a groove up and down, the intersection of the two grooves formation fixed station that stretches out up and down, be placed on the pedestal (14) by thermal sleeve (13) around the fixed station, and by bolt, electrothermal tube (10) places in the groove border of well heater (11) bottom.
8. utilize the petroleum products acid number automatic testing method of circumfluence method, it is characterized in that: right to use requires the petroleum products acid number automatic detection device of 1 ~ 7 each described circumfluence method to detect, and step is as follows:
Step 1001, beginning, power-on, automatic detection device enters duty;
Step 1002 is installed initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to the function setting flow process, and after setting was finished, automatic detection device carried out work according to setting;
Step 1004, the cleaning before judging whether to shut down, after automatic detection device work was finished, the cleaning before whether display prompts shuts down if can shut down and clean this moment, was then selected "Yes" by button, and then execution in step 1005; If do not need to clean, then select "No" by button, then execution in step 1006; Carry out next one test if desired, select " cancellation " by button, return step 1003;
Step 1005 is cleaned, and CPU control is cleaned titration cell (7) and internal pipeline;
Step 1006, shutdown, automatic detection device work finishes, automatically shutdown.
9. the petroleum products acid number automatic testing method that utilizes circumfluence method according to claim 8, it is characterized in that: the function setting flow process described in the step 1003 the steps include:
Step 2001, the interface initialization, the display interface of CPU carries out initialization;
Step 2002, CPU has judged whether button input, CPU is, and button scans, and whether the decision operation personnel carried out the instruction input by button, if there is not the button input, then proceeds key scan; If operating personnel have selected " instrument self checking " function by button, then execution in step 2003; As selected " test " function, and then execution in step 2004, if selected " parameter setting " function, then execution in step 2005, if selected " shutdown " then execution in step 2006;
Step 2003, instrument self checking, execution unit carries out status detection in the automatic detection device of CPU;
Step 2004 is tested, and CPU control automatic detection device is tested according to the process of the test flow process;
Step 2005, parameter is set, and operating personnel carry out the setting of test parameters again;
Step 2006, shutdown, power-off operation is carried out in CPU control.
10. the petroleum products acid number automatic testing method that utilizes circumfluence method according to claim 9, it is characterized in that: the process of the test flow process described in the step 2002 the steps include:
Step 3001 is cleaned for the first time, and CPU control peristaltic pump (17) extracts alcohol titration cell (7) inside and internal duct are cleaned, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump (17) was discharged equally;
Step 3002 is measured test products, and the product to be measured that CPU control peristaltic pump (17) extracts 10mL enters in the buret;
Step 3003, the unnecessary product to be measured of emptying, CPU control peristaltic pump (17) is discharged product to be measured unnecessary in the pipeline;
Step 3004, clean the second time, and CPU control peristaltic pump (17) extracts alcohol the cleaning second time is carried out in titration cell (7) inside and internal duct, and after cleaning was finished, the waste liquid of cleaning being finished by peristaltic pump (17) was discharged equally;
Step 3005 is injected product to be measured and extract, and CPU control peristaltic pump (17) injects the product to be measured of the 10mL in the buret in the titration cell (7), measures the extract of 50mL then equally by buret, injects equally in the titration cell (7);
Step 3006, heating, condensation, CPU control electrothermal tube (10) work, and by well heater (11) titration cell (7) is heated, in the process of heating, extract constantly evaporates, evaporation passes back into again in the titration cell (7) after entering condenser pipe, so circulation;
Step 3007, CPU judges whether product to be measured in the titration cell (7) and the mixed liquor of extract seethe with excitement, if seethe with excitement, then execution in step 3008, if step 3006 is returned in also not boiling;
Step 3008 begins to stir, and the work of CPU control magnetic stirring apparatus is stirred the mixed liquor in the titration cell (7), and mixing time is 5min;
Step 3009, inject indicator, titration syringe needle (3) dropwise splashes into indicator in titration cell (7), the grooved photoelectricity coupling (6) corresponding with this titration syringe needle (3) detected and calculated by CPU the quantity that splashes into this moment, reaches dosage and stops to splash into of indicator afterwards;
Step 3010, beginning titration, Photoelectric Detection also calculated, in titration cell (7), dropwise splash into neutralizing agent by another titration syringe needle (3), at this moment, the grooved photoelectricity coupling (6) corresponding with this titration syringe needle (3) detects the quantity that splashes into and concrete quantity is sent to CPU, and calculates by display screen by CPU and to show; The photoelectric detection system of CPU control is simultaneously started working, and detects the variation of the interior liquid color of separating pool (21);
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point then execution in step 3012, if the no show titration end-point is returned step 3010;
Step 3012, stop heating, titration, Photoelectric Detection and calculate, the titration syringe needle (3) that CPU control splashes into neutralizing agent stops to splash into neutralizing agent, stops to continue heating and stirring simultaneously, and passes through the final acid number of the data computation product to be measured of grooved photoelectricity coupling (6) transmission;
Step 3013, CPU judges whether and need print net result, prints if desired, execution in step 3014 is not if need to print execution in step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015 finishes, and process of the test finishes.
CN201310250142.9A 2013-06-22 2013-06-22 Device and method for automatically detecting acid value of petroleum product through reflux method Active CN103308469B (en)

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