CN103308469B - 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 PDFInfo
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- CN103308469B CN103308469B CN201310250142.9A CN201310250142A CN103308469B CN 103308469 B CN103308469 B CN 103308469B CN 201310250142 A CN201310250142 A CN 201310250142A CN 103308469 B CN103308469 B CN 103308469B
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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
Technical field
Utilize petroleum products acid number automatic detection device and the detection method of circumfluence method, belong to petroleum product analysis Instrument technology field.Be specifically related to a kind of circumfluence method that adopts detect petroleum products acid number, petroleum products acid number automatic detection device and the detection method of the function such as auto injection, automatic liquid-feeding, automatic gauge, automatically measurement, automatically cleaning, automatic drain can be completed.
Background technology
Petroleum products acid number is an important indicator of Check and Inspection petroleum products.When the acidity of carrying out petroleum products detects, first by the extract of a certain amount of product to be detected and corresponding proportion, then heat, indicator is added after boiling, and instillation neutralizing agent while carrying out constantly stirring to liquid, when the neutralizing agent added two lucky with the acid number when detected sample in and time, indicator color is undergone mutation, now stop adding neutralizing agent, the gauge then by calculating added neutralizing agent calculates the acid number of product to be detected.
In the prior art, carry out mainly adopting two kinds of methods when acid number detects to petroleum products: (1) is manually detected, and the defect of the method is intricate operation, and workload is large and error is larger; (2) automatically detected by automatic tester, the color being treated tracer liquid by light sensitive device is detected.But when using automatic testing method, if the vessel radius holding liquid to be detected is less, then inconvenience stirs liquid, there will be and stirs irregular phenomenon; If the radius of container is comparatively large, then current light sensation technology is difficult to detect through thicker container.The way generally adopted at present is after product to be detected and extract are fully mixed boiling, be drawn in the less container of another one radius and carry out in titration and test, but when making in this way, in the process extracted, one is the loss that there will be temperature, time particularly room temperature is lower, two is that the tube wall extracted can leave certain liquid, there will be larger measuring error equally.So, in short supply current technician, when labor intensive is large, invents and a kind ofly can realize the robotization of a series of process such as petroleum product acid value measuring apparatus automatic liquid-feeding, automatically measurements, automatic gauge, automatic cleaning and accurately detect that product acid number product to be measured becomes particularly important.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provides a kind of circumfluence method that adopts in same titration cell, automatically can complete high precision test higher the petroleum products acid number automatic detection device and the detection method that utilize circumfluence method.
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, comprise the titration cell of cup-shaped, be arranged on the stirring apparatus bottom titration cell and heating arrangement, and the titration apparatus be arranged on above titration cell, it is characterized in that: bottom described titration cell, side stretches out formation one separating pool, the both sides of separating pool are fixed with the photoelectric detection system be made up of photoemission cell and photoelectric receiving tube, and titration cell oral area is provided with the titration return be connected with titration cell inside.
The cylindrical structural of described separating pool to be diameter be 15 ~ 25mm, left and right sides trimming.
Described titration return comprises the buret and condenser pipe lower fixed hole that protrude from titration cell oral area upper surface, the upper coarse and lower fine right side being arranged at 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 simultaneously communicates with titration cell inside and adds discharging tube lower fixed hole, and buret and the condenser pipe lower fixed hole of described titration apparatus and titration cell oral area match.
Described buret is that two front and back are symmetrical arranged.
Described titration apparatus comprises and is fixed on two the titration syringe needles and two grooved photoelectricity couplings that titration covers, two grooved photoelectricity couplings to be fixed in the photoelectricity coupling pickup groove bottom titration lid and corresponding with two burets respectively, and titration syringe needle is from top to bottom through titration lid and the corresponding titration syringe needle jack being arranged on grooved photoelectricity coupling center that inserts is placed in corresponding buret;
The upper surface of titration lid is disposed with fixed orifice on condenser pipe from back to front, fixed orifice and add fixed orifice on discharging tube on temperature sensor, level be symmetrically respectively provided with a titration syringe needle fixed orifice and the wire fairlead in titration syringe needle fixed orifice both sides between fixed orifice on fixed orifice and condenser pipe on temperature sensor, the front end of each titration syringe needle fixed orifice is provided with a titration syringe needle pickup groove communicated with it;
Fixed orifice and add fixed orifice on discharging tube respectively with the condenser pipe lower fixed hole of titration cell oral area, temperature sensor lower fixed hole with add discharging tube lower fixed hole and be connected on fixed orifice, temperature sensor on 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 being placed on titration cell inside and the magnetic agitation motor be fixed on below titration cell.
Described heating arrangement comprises electrothermal tube and well heater, well heater is the sheet metal being respectively provided with a groove up and down, the intersection of upper and lower two grooves stretches out formation fixed station, be placed on pedestal by thermal sleeve around fixed station, and be bolted, electrothermal tube is placed in the groove border of heater base.
Described heating arrangement comprises electrothermal tube and well heater, well heater is the sheet metal being respectively provided with a groove up and down, the intersection of upper and lower two grooves stretches out formation fixed station, be placed on pedestal by thermal sleeve around fixed station, and be bolted, electrothermal tube is placed 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, start, after electric power starting, this automatic detection device enters duty;
Step 1002, device initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to function setting flow process, and after having set, this automatic detection device carries out work according to setting;
Step 1004, judges whether to need the cleaning before shutting down, after the work of this automatic detection device completes, display prompts whether shut down before cleaning, if now can shut down and clean, then select "Yes" by button, then perform step 1005; If do not need to clean, then select "No" by button, then perform step 1006; If need to carry out next one test, select " cancellation " by button, return step 1003;
Step 1005, cleaning, CPU controls to clean titration cell and internal pipeline;
Step 1006, shutdown, the work of this automatic detection device is complete, automatic shutdown.
Function setting flow process described in step 1003, the steps include:
Step 2001, interface initialization, CPU carries out initialization to display interface;
Step 2002, CPU has judged whether key-press input, and CPU scans button, and judges whether operating personnel have carried out instruction input by button, if do not have key-press input, then proceed key scan; If operating personnel have selected " instrument self checking " function by button, then perform step 2003; As have selected " test " function, then performing step 2004, if having selected " setting parameter " function, then performing step 2005, if having selected " shutdown ", perform step 2006;
Step 2003, instrument self checking, CPU carries out the detection of state to execution unit in this automatic detection device;
Step 2004, tests, and CPU controls this automatic detection device and tests according to process of the test flow process;
Step 2005, setting parameter, operating personnel re-start the setting of test parameters;
Step 2006, shutdown, CPU controls to carry out power-off operation.
Process of the test flow process described in step 2004, the steps include:
Step 3001, first time cleaning, CPU controls peristaltic pump pumps alcohol and cleans titration cell inside and internal duct, after having cleaned, is discharged by the waste liquid cleaned equally by peristaltic pump;
Step 3002, measures test products, and CPU controls in the product introduction buret to be measured of peristaltic pump pumps 10mL;
Step 3003, emptying unnecessary product to be measured, CPU controls peristaltic pump and is discharged by product to be measured unnecessary in pipeline;
Step 3004, second time cleaning, CPU controls peristaltic pump pumps alcohol and carries out second time cleaning to titration cell inside and internal duct, after having cleaned, is discharged by the waste liquid cleaned equally by peristaltic pump;
Step 3005, injects product to be measured and extract, and CPU controls peristaltic pump and injects in titration cell by product to be measured for the 10mL in buret, the then same extract being measured 50mL by buret, in same injection titration cell;
Step 3006, heating, condensation, CPU controls electrothermal tube work, and is heated titration cell by well heater, and in the process of heating, extract constantly evaporates, and evaporation passes back into again in titration cell after entering condenser pipe, so circulates;
Step 3007, CPU judges whether the mixed liquor of product to be measured in titration cell and extract seethes with excitement, if seethed with excitement, then performs step 3008, if also do not seethed with excitement, returns step 3006;
Step 3008, start to stir, CPU controls magnetic stirring apparatus work, and stir the mixed liquor in titration cell, mixing time is 5min;
Step 3009, inject indicator, titration syringe needle dropwise instills indicator in titration cell, and the quantity of now corresponding with this titration syringe needle symplectic instillation of grooved photoelectricity carries out detecting and being calculated by CPU, stops the instillation of indicator after reaching dosage;
Step 3010, start titration, Photoelectric Detection calculating, in titration cell, dropwise neutralizing agent is instilled by another titration syringe needle, now, the quantity of the grooved photoelectricity symplectic instillation corresponding with this titration syringe needle carries out detecting and concrete quantity is sent to CPU, and is undertaken calculating being shown by display screen by CPU; The photoelectric detection system of CPU control is simultaneously started working, and detects the change of liquid color in separating pool;
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point, performs step 3012, if the titration end-point of arrival, returns step 3010;
Step 3012, stops heating, titration, Photoelectric Detection calculating, and the titration syringe needle that CPU controls instillation neutralizing agent stops instillation neutralizing agent, stops continuing heating and stirring simultaneously, and calculates the final acid number of product to be measured by the data that grooved photoelectricity coupling transmits;
Step 3013, CPU judges whether to need to print net result, if need to print, performs step 3014, if do not need to print, performs step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015, terminate, process of the test terminates.
Compared with prior art, of the present invention had beneficial effect is:
1, the steps such as cleaning, liquid feeding, heating, stirring, measurement and metering can automatically be completed in same titration cell by automatic detection device of the present invention, solve after product to be detected and extract fully mix boiling by prior art, need be drawn in the less container of another one radius and carry out in titration and test, cause temperature inaccurate because temperature declines in extraction process, and the tube wall extracted can leave certain liquid and cause the problem that measuring error is larger thus.Really achieve high precision test.
2, the cylindrical structural of separating pool to be diameter be 15 ~ 25mm, left and right sides trimming, thus make light better through the liquid in separating pool, make detection more accurate.
3, devise the matching used titration lid with titration cell, adopt the infusion volume of the symplectic neutralizing agent of grooved photoelectricity and indicator to calculate, what product acid number to be detected was calculated is more accurate.
4, according to the characteristic of indicator, have employed the photoemission cell sending blue light, make more light can through the liquid in separating pool.
5, have employed circumfluence method, thus in heating process, the extract evaporated is back in titration cell again, thus avoids the consumption of the extract caused because of heating, make the result of calculating more accurate.
6, have employed the design of condenser pipe, the drain evaporation of extract in titration cell can be reduced to the full extent.
7, have employed single-chip microcomputer to control the duty of complete machine as CPU, duty is more reliable.
8, the light that photoemission cell sends is blue light, with just complete in time indicator color identical, thus easier change light intensity being detected of photoelectric receiving tube can be made.
9, structure is simple, and the parts adopted are universal component, and reliability is high and be easy to change.
Accompanying drawing explanation
Fig. 1 is the petroleum products acid number automatic detection device structural representation utilizing 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 utilizing circumfluence method.
Fig. 4 is the petroleum products acid number automatic detection device titration cell right view utilizing circumfluence method.
Fig. 5 is the petroleum products acid number automatic detection device titration cell vertical view utilizing circumfluence method.
Fig. 6 is the main pseudosection of petroleum products acid number automatic detection device titration lid utilizing circumfluence method.
Fig. 7 is the petroleum products acid number automatic detection device titration lid vertical view utilizing circumfluence method.
Fig. 8 is the petroleum products acid number automatic testing method detecting step process flow diagram utilizing circumfluence method.
Fig. 9 is the petroleum products acid number automatic testing method function setting process flow diagram utilizing circumfluence method.
Figure 10 is the petroleum products acid number automatic testing method process of the test process flow diagram utilizing circumfluence method.
Wherein: 1, temperature sensor 2, photoelectricity coupling wire 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 temperature sensor, wire fairlead 28, screw hole 29, titration syringe needle fixed orifice 30, photoelectricity coupling pickup groove 31, fixed orifice 32 on condenser pipe, titration syringe needle pickup groove 33, add fixed orifice on discharging tube.
Embodiment
Fig. 1 ~ 10 are most preferred embodiments of the present invention, and below in conjunction with accompanying drawing 1 ~ 10, the present invention will be further described.
As shown in Figure 1 and 2, the petroleum products acid number automatic detection device (hereinafter referred to as automatic detection device) of circumfluence method that utilizes of the present invention forms primarily of following components: titration cell 7 and coordinate titration apparatus, photoelectric detection system, stirring apparatus, heating arrangement, backflow refrigerating plant condenser pipe being carried out to refrigeration and the input-output unit installed with titration cell 7.Wherein input-output unit comprises button, the display show duty and the printing equipment printed net result that practical function is selected.The duty of whole pick-up unit is controlled by control circuit, and it is the single-chip microcomputer of STM32F1032ET carries out function realization as CPU that control circuit have employed model.
Heating arrangement comprises electrothermal tube 10 and well heater 11.Well heater 11 is rectangular metal device, and its top and bottom are respectively provided with a circular groove, and titration cell 7 is placed in the groove at its top.Fixed station is protruding with at the intersection of upper and lower two grooves, thermal sleeve 13 is placed with below fixed station, after thermal sleeve 13 installation, by screw bolt passes fixed station and thermal sleeve 13, well heater 11 is fixed to above pedestal 14, after fixedly completing, the groove bottom well heater 11 is embedded in pedestal 14.Electrothermal tube 10 is positioned at the groove border bottom well heater 11.
Stirring apparatus comprises the magnetic stirring apparatus be positioned at below well heater 11, and magnetic agitation motor 12 top in magnetic stirring apparatus is connected with magnetic force rotary head 9 bottom, and the top of magnetic force rotary head 9 is placed in the groove bottom well heater 11.It is inner that the magnetic stir bar 8 be used in combination with magnetic force rotary head 9 is positioned over titration cell 7.
Titration apparatus comprise with titration cell 7 with the use of two the grooved photoelectricity couplings 6 being arranged on two titration syringe needles 3 on titration lid 4 and matching with respectively at each titration syringe needle 3.
Titration lid 4 is rectangular block shape, is placed on above titration cell 7, and its bottom centre position both sides are respectively provided with a groove, and each groove internal fixtion has a grooved photoelectricity coupling 6, is placed with a seal gasket 15 between each grooved photoelectricity coupling 6 and titration lid 4.The two photoelectricity coupling wires 2 be connected with grooved photoelectricity coupling 6 are drawn from titration lid 4 upper surface.The equal correspondence of each grooved photoelectricity coupling 6 is provided with a titration syringe needle 3, two titration syringe needles 3 are from top to bottom through titration lid 4, the bottom of each titration syringe needle 3 is positioned at corresponding grooved photoelectricity coupling 6 center, and grooved photoelectricity coupling 6 is for detecting the quantity of the liquid oozed from titration syringe needle 3.After titration lid 4 covers above titration cell 7, two burets 22 on titration cell 7 are 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 is placed on the bottom of titration cell 7 from top to bottom simultaneously successively through titration lid 4 and titration cell 7 with adding discharging tube 16, add on discharging tube 16 and be provided with peristaltic pump 17.
Photoelectric detection system comprises photoemission cell 18 and photoelectric receiving tube 19, and photoemission cell 18 and photoelectric receiving tube 19 are secured by bolts on the backboard 20 at its back side simultaneously.Extend from titration cell 7 bottom rear and have separating pool 21, separating pool 21 is between photoemission cell 18 and photoelectric receiving tube 19, so that photoemission cell 18 and photoelectric receiving tube 19 detect the color change in separating pool 21.
Temperature sensor 1, photoemission cell 18 and photoelectric receiving tube 19 are connected with CPU simultaneously.
As shown in Fig. 3 ~ 5, titration cell 7 is glass cup-like containers, treats testing product therein and carries out stirring titration operation.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 for diameter be the cylindrical structural of 15 ~ 25mm, left and right sides trimming.Be convenient to photoelectric detection system detect the liquid in it.
The oral area of titration cell 7 is half sealing design, has condenser pipe lower fixed hole 23, be disposed with temperature sensor lower fixed hole 24 and add discharging tube lower fixed hole 25 on the left of condenser pipe lower fixed hole 23 on the right side of its oral area.Temperature sensor lower fixed hole 24 is provided with two burets 22 with the symmetria bilateralis adding discharging tube lower fixed hole 25, and buret 22 protrudes from the upper surface of titration cell 7 oral area.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 communicated with titration cell 7 inside, and the part that buret 22 and condenser pipe lower fixed hole 23 are in titration cell 7 oral area is upper coarse and lower fine conical design, buret 22 is upper inferior design slightly above the part of titration cell 7 oral area.
As shown in Fig. 6 ~ 7, titration lid 4 designs for cuboid, and the two bottom sides symmetry of titration lid 4 is respectively provided with the photoelectricity coupling pickup groove 30 of a rectangle.Each photoelectricity coupling pickup groove 30 left and right sides edge is respectively provided with a screw hole 28.
The upper surface rear portion of titration lid 4 is provided with fixed orifice 31 on condenser pipe, on condenser pipe, fixed orifice 31 front to be disposed with on temperature sensor fixed orifice 26 and to add fixed orifice 33 on discharging tube, fixed orifice 26 and add fixed orifice 33 on discharging tube and be each side symmetrically arranged with a titration syringe needle fixed orifice 29 on temperature sensor, each titration syringe needle fixed orifice 29 is each side symmetrically arranged with a wire fairlead 27, and the front end of each titration syringe needle fixed orifice 29 is provided with the titration syringe needle pickup groove 32 that extends to titration lid 4 front end.The wire fairlead 27 of each group titration syringe needle fixed orifice 29 and its both sides correspond to the photoelectricity coupling pickup groove 30 be positioned at bottom titration lid 4, and each titration syringe needle fixed orifice 29 is all positioned at the center of corresponding photoelectricity coupling pickup groove 30.Temperature sensor lower fixed hole 24 and to add on discharging tube fixed orifice 33 side by side between the photoelectricity coupling pickup groove 30 of two, left and right.
Fixed orifice 26 and add fixed orifice 33 on discharging tube and be the through hole of upper and lower UNICOM on fixed orifice 31, wire fairlead 27, temperature sensor on above-mentioned titration syringe needle fixed orifice 29, condenser pipe.Wherein on condenser pipe, fixed orifice 31 is upper coarse and lower fine conical through-hole; Two titration syringe needle fixed orifices 29 are the through hole of upper coarse and lower fine step cutting pattern shape.On temperature sensor, fixed orifice 26 is similarly the through hole of upper coarse and lower fine step cutting pattern shape.
As shown in Fig. 6 ~ 7, two grooved photoelectricity couplings 6 are placed in the photoelectricity coupling pickup groove 30 bottom titration lid 4 respectively, a seal gasket 15 is provided with between the grooved photoelectricity coupling 6 of every side and titration lid 4, and by both sides totally four holding screws 5 screw in corresponding screw hole 28, the seal gasket 15 of two grooved photoelectricity couplings 6 and top is fixed in the photoelectricity coupling pickup groove 30 of corresponding side.The grooved photoelectricity coupling 6 of every side is all connected with two photoelectricity coupling wires 2, two photoelectricity coupling wires 2 of every side are upwards drawn above titration lid 4 through seal gasket 15 and wire fairlead 27 successively.A titration syringe needle 3 is placed with all from top to bottom in the titration syringe needle fixed orifice 29 of every side.Grooved photoelectricity coupling 6 two is connected with CPU respectively by corresponding photoelectricity coupling wire 2.
In the present invention, what titration syringe needle 3 adopted is the common transfusion bottle syringe needle that matches with transfusion bottle, the plastic end that such transfusion bottle syringe needle comprises upper end and the thinner metal needle of drawing from plastic end, and plastic end side is provided with a plastic handles.By this titration syringe needle 3 from top to bottom through titration syringe needle fixed orifice 29, the plastics section that titration syringe needle 3 upper end is thicker and matching from the thinner metal needle design upper coarse and lower fine with titration syringe needle fixed orifice 29 that plastic end is drawn is installed, and the plastic handles above titration syringe needle 3 is stuck in corresponding titration syringe needle pickup groove 32, is fixed by titration syringe needle 3.After the titration syringe needle 3 of every side fixedly completes, the fluid place, bottom of titration syringe needle 3 is all in the center of corresponding grooved photoelectricity coupling 6.
After titration apparatus fixedly completes, may correspond to the top of lid to titration cell 7.Now, two burets 22 outstanding on titration cell 7 are corresponding with a grooved photoelectricity coupling 6 respectively, and snapping between corresponding grooved photoelectricity coupling 6, the bottom being positioned at the titration syringe needle 3 of grooved photoelectricity coupling 6 center of every side all enters corresponding buret 22 inside.Be arranged at simultaneously on titration lid 4 to add on discharging tube fixed orifice 26 on fixed orifice 31 on fixed orifice 33, condenser pipe and temperature sensor respectively be arranged on titration cell 7 oral area to add discharging tube lower fixed hole 25, condenser pipe lower fixed hole 23 and temperature sensor lower fixed hole 24 corresponding, and add discharging tube 16 successively through to add on discharging tube fixed orifice 33 and add discharging tube lower fixed hole 25, temperature sensor 1 stretches in titration cell 7 through fixed orifice 26, temperature sensor lower fixed hole 24 on temperature sensor successively, is positioned at the bottom of titration cell 7.Condenser pipe is positioned at titration cell 7 through its lower end after fixed orifice 31 on condenser pipe and condenser pipe lower fixed hole 23 successively.
After condenser pipe installation, the backflow refrigerating plant in automatic detection device of the present invention is connected with the refrigerant circulation mouth of pipe be arranged on above and below condenser pipe respectively, and condensing agent within it circulates.Condenser pipe carries out condensation to the extract be evaporated in condenser pipe, and vaporous extract condenses into liquid through the condensation of condenser pipe at the inwall of condenser pipe and is back in titration cell 7, to ensure that the dosage of extract remains unchanged.Backflow refrigerating plant is more ripe prior art, and can be realized by the mode of water circulation, also can pass through compressed refrigerant, the mode of being undertaken freezing by cold-producing medium realizes.
In automatic detection device of the present invention, after neutralization is completed to the product to be measured in titration cell 7, can calculate the acid number of product to be measured, and be printed by printing device.
Be illustrated in figure 8 the petroleum products acid number automatic testing method detecting step process flow diagram utilizing circumfluence method of the present invention, its concrete steps are:
Step 1001, start, after electric power starting, this automatic detection device enters duty;
Step 1002, device initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to function setting flow process, and after having set, this automatic detection device carries out work according to setting;
Step 1004, judges whether to need the cleaning before shutting down, after the work of this automatic detection device completes, display prompts whether shut down before cleaning, if now can shut down and clean, then select "Yes" by button, then perform step 1005; If do not need to clean, then select "No" by button, then perform step 1006; If need to carry out next one test, select " cancellation " by button, return step 1003;
Step 1005, cleaning, CPU controls to clean titration cell and internal pipeline;
Step 1006, shutdown, the work of this automatic detection device is complete, automatic shutdown.
Be illustrated in figure 9 the petroleum products acid number automatic testing method function setting process flow diagram utilizing circumfluence method of the present invention, its concrete steps are:
Step 2001, interface initialization, CPU carries out initialization to display interface;
Step 2002, CPU has judged whether key-press input, and CPU scans button, and judges whether operating personnel have carried out instruction input by button, if do not have key-press input, then proceed key scan; If operating personnel have selected " instrument self checking " function by button, then perform step 2003; As have selected " test " function, then performing step 2004, if having selected " setting parameter " function, then performing step 2005, if having selected " shutdown ", perform step 2006;
Step 2003, instrument self checking, CPU carries out the detection of state to execution unit in this automatic detection device;
Step 2004, tests, and CPU controls this automatic detection device and tests according to process of the test flow process;
Step 2005, setting parameter, operating personnel re-start the setting of test parameters;
Step 2006, shutdown, CPU controls to carry out power-off operation.
The state-detection of execution unit mainly comprises the closedown situation of solenoid valve in pipeline and the running status of pump.
Be the petroleum products acid number automatic testing method process of the test process flow diagram utilizing circumfluence method of the present invention as shown in Figure 10, its concrete steps are:
Step 3001, first time cleaning, CPU control peristaltic pump 17 extracts alcohol and cleans titration cell 7 inside and internal duct, and after having cleaned, the waste liquid that will have been cleaned by peristaltic pump 17 is equally discharged;
Step 3002, measures test products, and CPU controls peristaltic pump 17 and extracts in the product introduction buret to be measured of 10mL;
Step 3003, emptying unnecessary product to be measured, CPU controls peristaltic pump 17 and is discharged by product to be measured unnecessary in pipeline;
Step 3004, second time cleaning, CPU control peristaltic pump 17 extracts alcohol and carries out second time cleaning to titration cell 7 inside and internal duct, after having cleaned, is discharged by the waste liquid cleaned equally by peristaltic pump 17;
Step 3005, injects product to be measured and extract, and CPU controls peristaltic pump 17 and injects in titration cell 7 by product to be measured for the 10mL in buret, the then same extract being measured 50mL by buret, in same injection titration cell 7;
Step 3006, heating, condensation, CPU controls electrothermal tube 10 and works, and is heated by well heater 11 pairs of titration cells 7, and in the process of heating, extract constantly evaporates, and evaporation refluxes as in titration cell 7 again after entering condenser pipe, so circulates;
Step 3007, CPU judges whether the mixed liquor of product to be measured in titration cell 7 and extract seethes with excitement, if seethed with excitement, then performs step 3008, if also do not seethed with excitement, returns step 3006;
Step 3008, start to stir, CPU controls magnetic stirring apparatus work, and stir the mixed liquor in titration cell 7, mixing time is 5min;
Step 3009, inject indicator, titration syringe needle 3 dropwise instills indicator in titration cell 7, and now corresponding with this titration syringe needle 3 grooved photoelectricity coupling 6 is detected the quantity instilled and calculated by CPU, stops the instillation of indicator after reaching dosage;
Step 3010, start titration, Photoelectric Detection calculating, in titration cell 7, dropwise neutralizing agent is instilled by another titration syringe needle 3, now, the grooved photoelectricity coupling 6 corresponding with this titration syringe needle 3 detects the quantity instilled and concrete quantity is sent to CPU, and is undertaken calculating being shown by display screen by CPU; The photoelectric detection system of CPU control is simultaneously started working, and detects the change of liquid color in separating pool 21;
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point, performs step 3012, if the titration end-point of arrival, returns step 3010;
Step 3012, stop heating, titration, Photoelectric Detection calculating, the titration syringe needle 3 that CPU controls instillation neutralizing agent stops instillation neutralizing agent, stops continuing heating and stirring simultaneously, and calculates the final acid number of product to be measured by the data of grooved photoelectricity coupling 6 transmission;
Step 3013, CPU judges whether to need to print net result, if need to print, performs step 3014, if do not need to print, performs step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015, terminate, process of the test terminates.
In this process of the test, adopt alcohol as extract.After starting to heat, temperature sensor 1 carries out temperature detection, and real time temperature is passed to CPU, and CPU calculates temperature, when calculating temperature and significant change no longer occurring, then represents that the mixed liquor in titration cell 7 reaches fluidized state.
Specific works process is as follows: after the start of this automatic detection device, that first automatically carries out cpu clock and peripheral apparatus carries out initialization, then operating personnel carry out function setting, if have selected " instrument self checking " or " setting parameter " function, then this automatic detection device carries out corresponding function automatically, if have selected " test " function, then carry out the test of product to be measured.
First this automatic detection device injects alcohol by peristaltic pump 17 in pipeline and titration cell 7, carries out first time and rinses, automatically discharged by waste alcohol after having rinsed.Then product to be measured is pumped in the buret that dosage is 10mL by peristaltic pump 17, then unnecessary product to be measured discharged, and carry out second time and clean.Then through adding discharging tube 16, product to be measured for the 10mL in buret being injected in titration cell 7 under the effect of peristaltic pump 17, being divided the extract alcohol measuring common 50mL for five times by buret then equally, injecting in titration cell 7 through adding discharging tube 16.
Now CPU control heater 11 pairs of titration cells 7 heat.Now temperature sensor 1 starts the temperature detecting liquid in titration cell 7, and the temperature value detected is sent to CPU, that CPU when detecting in titration cell 7 mixed liquor and be in fluidized state, CPU controls magnetic stirring apparatus and stirs the mixed liquor in titration cell 7, and mixing time is 5 minutes.Then in titration cell 7, a certain amount of indicator is instilled by a titration syringe needle 3, in indicator titration process, the grooved photoelectricity coupling 6 corresponding with this titration syringe needle 3 detects the amount of the indicator instilled, after indicator has instilled, stop the instillation of indicator, and begin through another titration syringe needle 3 instill neutralizing agent in titration cell 7.
In the process of neutralizing agent instillation, the dripping of neutralizing agent of the grooved photoelectricity coupling 6 real time record instillation of corresponding side counts, and the photoemission cell 18 being simultaneously positioned at separating pool 21 side is luminous, and corresponding photoelectric receiving tube 19 receives the light that photoemission cell 18 sends.When the amount that neutralizing agent adds and product to be detected acid number just in and time, the color change of the indicator in it, the light intensity of light that now photoelectric receiving tube 19 receives changes, and controls titration syringe needle 3 and stops continuing instillation neutralizing agent.Well heater 11 and magnetic stirring apparatus quit work simultaneously.In whole neutralization reaction process, CPU calculates the quantity of the neutralizing agent of instillation in real time, and shows over the display.
Last CPU calculates the acid number in product to be detected by the gauge of the neutralizing agent instilled.In whole process of the test, extract constantly evaporates and enters in the condenser pipe be arranged on above titration lid 4, and after condenser pipe cooling, backflow is as in titration cell 7, ensures that the amount of extract in titration cell 7 remains unchanged.
After having tested, whether operating personnel can select test findings to be printed, and then this automatic detection device judges whether shutdown and the cleaning before whether shutting down, and after above step completes, this is completed.
In the present embodiment, what in titration cell 7, liquid carried out that thermometric temperature sensor 1 adopts is 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 BTB indicator.Because during neutralizing agent just completes with product to be detected and time, the color change of this indicator is blue, so the light that photoemission cell 18 sends is for blue, can when indicator becomes blueness through stronger light, what photoelectric receiving tube 19 adopted is commercially available common phototriode.
What condenser pipe adopted is common spherical condensation tube, can carry out condensation in it by condensate water or other cold-producing mediums.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (8)
1. utilize the petroleum products acid number automatic detection device of circumfluence method, comprise the titration cell (7) of cup-shaped, be arranged on stirring apparatus and the heating arrangement of titration cell (7) bottom, and be arranged on the titration apparatus of titration cell (7) top, it is characterized in that: side, described titration cell (7) bottom stretches out formation one separating pool (21), the both sides of separating pool (21) are fixed with the photoelectric detection system be made up of photoemission cell (18) and photoelectric receiving tube (19), and titration cell (7) oral area is provided with the titration return be connected with titration cell (7) inside.
2. the petroleum products acid number automatic detection device utilizing circumfluence method according to claim 1, is characterized in that: described separating pool (21) for diameter be the cylindrical structural of 15 ~ 25mm, left and right sides trimming.
3. the petroleum products acid number automatic detection device utilizing circumfluence method according to claim 1, it is characterized in that: described titration return comprises the buret (22) and condenser pipe lower fixed hole (23) that protrude from titration cell (7) oral area upper surface, the upper coarse and lower fine right side being 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 simultaneously communicates with titration cell (7) inside and adds discharging tube lower fixed hole (25), buret (22) and the condenser pipe lower fixed hole (23) of described titration apparatus and titration cell (7) oral area match.
4. the petroleum products acid number automatic detection device utilizing circumfluence method according to claim 3, is characterized in that: described buret (22) is that two front and back are symmetrical arranged.
5. the petroleum products acid number automatic detection device utilizing circumfluence method according to claim 1 or 3, it is characterized in that: described titration apparatus comprises and is fixed on two titration syringe needles (3) on titration lid (4) and two grooved photoelectricity couplings (6), two grooved photoelectricity couplings (6) are fixed in the photoelectricity coupling pickup groove (30) bottom titration lid (4) also corresponding with two burets (22) respectively, titration syringe needle (3) passes titration lid (4) from top to bottom and the corresponding titration syringe needle jack being arranged on grooved photoelectricity coupling (6) center that inserts is placed in corresponding buret (22),
The upper surface of titration lid (4) is disposed with fixed orifice on condenser pipe (31) from back to front, fixed orifice (26) and add fixed orifice on discharging tube (33) on temperature sensor, level be symmetrically respectively provided with a titration syringe needle fixed orifice (29) and the wire fairlead (27) in titration syringe needle fixed orifice (29) both sides between fixed orifice (31) on fixed orifice (26) and condenser pipe on temperature sensor, the front end of each titration syringe needle fixed orifice (29) is provided with a titration syringe needle pickup groove (32) communicated with it;
Fixed orifice (26) and add fixed orifice on discharging tube (33) respectively with the condenser pipe lower fixed hole (23) of titration cell (7) oral area, temperature sensor lower fixed hole (24) with add discharging tube lower fixed hole (25) and be connected on fixed orifice (31), temperature sensor on described condenser pipe; Each titration syringe needle fixed orifice (29) is connected with the center of a photoelectricity coupling pickup groove (30) respectively.
6. the petroleum products acid number automatic detection device utilizing circumfluence method according to claim 1, it is characterized in that: described stirring apparatus is magnetic stirring apparatus, comprise the magnetic agitation motor (12) being placed on the inner magnetic stir bar (8) of titration cell (7) and being fixed on titration cell (7) below.
7. the petroleum products acid number automatic detection device utilizing 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 the sheet metal being respectively provided with a groove up and down, the intersection of upper and lower two grooves stretches out formation fixed station, be placed on pedestal (14) by thermal sleeve (13) around fixed station, and be bolted, electrothermal tube (10) is placed 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: use the petroleum products acid number automatic detection device of circumfluence method described in any one of claim 1 ~ 7 to detect, step is as follows:
Step 1001, start, power-on, automatic detection device enters duty;
Step 1002, device initialization, carries out the initial work of cpu clock and peripheral hardware;
Step 1003, function setting, operating personnel carry out function setting according to function setting flow process, and after having set, automatic detection device carries out work according to setting;
Step 1004, judges whether to need the cleaning before shutting down, after automatic detection device work completes, display prompts whether shut down before cleaning, if now can shut down and clean, then select "Yes" by button, then perform step 1005; If do not need to clean, then select "No" by button, then perform step 1006; If need to carry out next one test, select " cancellation " by button, return step 1003;
Step 1005, cleaning, CPU controls to clean titration cell (7) and internal pipeline;
Step 1006, shutdown, automatic detection device work is complete, automatic shutdown;
Function setting flow process described in step 1003, the steps include:
Step 2001, interface initialization, CPU carries out initialization to display interface;
Step 2002, CPU has judged whether key-press input, and CPU scans button, and judges whether operating personnel have carried out instruction input by button, if do not have key-press input, then proceed key scan; If operating personnel have selected " instrument self checking " function by button, then perform step 2003; As have selected " test " function, then performing step 2004, if having selected " setting parameter " function, then performing step 2005, if having selected " shutdown ", perform step 2006;
Step 2003, instrument self checking, CPU carries out the detection of state to execution unit in automatic detection device;
Step 2004, tests, and CPU controls automatic detection device and tests according to process of the test flow process;
Step 2005, setting parameter, operating personnel re-start the setting of test parameters;
Step 2006, shutdown, CPU controls to carry out power-off operation;
Process of the test flow process described in step 2004, the steps include:
Step 3001, first time cleaning, CPU controls peristaltic pump (17) extraction alcohol and cleans titration cell (7) inside and internal duct, after having cleaned, is discharged by the waste liquid cleaned equally by peristaltic pump (17);
Step 3002, measures test products, and CPU controls peristaltic pump (17) and extracts in the product introduction buret to be measured of 10mL;
Step 3003, emptying unnecessary product to be measured, CPU controls peristaltic pump (17) and is discharged by product to be measured unnecessary in pipeline;
Step 3004, second time cleaning, CPU controls peristaltic pump (17) extraction alcohol and carries out second time cleaning to titration cell (7) inside and internal duct, after having cleaned, is discharged by the waste liquid cleaned equally by peristaltic pump (17);
Step 3005, injects product to be measured and extract, and CPU controls peristaltic pump (17) and injected in titration cell (7) by product to be measured for the 10mL in buret, and the then same extract being measured 50mL by buret, injects in titration cell (7) equally;
Step 3006, heating, condensation, CPU controls 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 titration cell (7) after entering condenser pipe, so circulates;
Step 3007, CPU judges whether the mixed liquor of product to be measured in titration cell (7) and extract seethes with excitement, if seethed with excitement, then performs step 3008, if also do not seethed with excitement, returns step 3006;
Step 3008, start to stir, CPU controls magnetic stirring apparatus work, and stir the mixed liquor in titration cell (7), mixing time is 5min;
Step 3009, inject indicator, titration syringe needle (3) dropwise instills indicator in titration cell (7), and now corresponding with this titration syringe needle (3) grooved photoelectricity coupling (6) is detected the quantity instilled and calculated by CPU, stops the instillation of indicator after reaching dosage;
Step 3010, start titration, Photoelectric Detection calculating, in titration cell (7), dropwise neutralizing agent is instilled by another titration syringe needle (3), now, the grooved photoelectricity coupling (6) corresponding with this titration syringe needle (3) detects the quantity instilled and concrete quantity is sent to CPU, and is undertaken calculating being shown by display screen by CPU; The photoelectric detection system of CPU control is simultaneously started working, and detects the change of separating pool (21) interior liquid color;
Step 3011, CPU judges whether to arrive titration end-point, if reach titration end-point, performs step 3012, if the titration end-point of arrival, returns step 3010;
Step 3012, stop heating, titration, Photoelectric Detection calculating, the titration syringe needle (3) that CPU controls instillation neutralizing agent stops instillation neutralizing agent, stops continuing heating and stirring simultaneously, and calculates the final acid number of product to be measured by the data that grooved photoelectricity coupling (6) transmits;
Step 3013, CPU judges whether to need to print net result, if need to print, performs step 3014, if do not need to print, performs step 3015;
Step 3014, print result, printing equipment prints net result;
Step 3015, terminate, process of the test terminates.
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| CN109781646B (en) * | 2019-03-15 | 2021-05-04 | 中世沃克(天津)科技发展股份有限公司 | Full-automatic ultraviolet aquatic oil detector |
| CN112303813B (en) * | 2020-09-24 | 2021-09-24 | 青岛海信日立空调系统有限公司 | Air conditioner and air conditioner defrosting method |
| CN112903905B (en) * | 2021-01-26 | 2024-01-12 | 山东惠工电气股份有限公司 | Automatic acid value sampling and weighing device by full-automatic reflux method |
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| JPH01165938A (en) * | 1987-12-23 | 1989-06-29 | Ebara Infilco Co Ltd | Detecting method and apparatus of ph |
| JPH01282450A (en) * | 1988-05-10 | 1989-11-14 | G R:Kk | Analysis container |
| CN2166445Y (en) * | 1993-08-17 | 1994-05-25 | 李有胜 | COD automatic analysis instrument |
| JP2008197044A (en) * | 2007-02-15 | 2008-08-28 | Sumitomo Metal Mining Co Ltd | Pretreatment method for moisture determination in paste and moisture determination method |
| JP5045333B2 (en) * | 2007-09-21 | 2012-10-10 | 東亜ディーケーケー株式会社 | Titration device |
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Address after: 255086 No. 131, Zibo hi tech Zone, Shandong, China Patentee after: Shandong Ketong Electric Technology Co. Ltd Address before: 255086, No. 126, Tai Mo Road, hi tech Zone, Shandong, Zibo Patentee before: Zibo Ketong Electrical Technology Co., Ltd. |