CN113495070B - Full-automatic pretreatment color titration analyzer and use method thereof - Google Patents
Full-automatic pretreatment color titration analyzer and use method thereof Download PDFInfo
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- CN113495070B CN113495070B CN202111003143.4A CN202111003143A CN113495070B CN 113495070 B CN113495070 B CN 113495070B CN 202111003143 A CN202111003143 A CN 202111003143A CN 113495070 B CN113495070 B CN 113495070B
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- 230000029087 digestion Effects 0.000 claims abstract description 61
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000010619 multiway switching Methods 0.000 claims description 74
- 238000002347 injection Methods 0.000 claims description 24
- 239000007924 injection Substances 0.000 claims description 24
- 230000002572 peristaltic effect Effects 0.000 claims description 23
- 239000002699 waste material Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/02—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
- G01N35/04—Details of the conveyor system
Abstract
The invention discloses a full-automatic pretreatment color titration analyzer and a use method thereof, wherein the full-automatic pretreatment color titration analyzer comprises a base and a bracket arranged on the base, a titration cup placement position and a digestion tube mounting frame are arranged on the bracket, and a temperature-controllable heating device is arranged below the digestion tube mounting frame; the device also comprises a liquid path flow path system, a control system and a detection system which are arranged on the bracket, wherein the liquid path flow path system and the detection system are connected with the control system, and the detection system is used for controlling the circulation of the reagent in the liquid path flow path system and realizing the titration of the reagent in the titration cup at the position where the titration cup is placed. In addition, the invention also discloses a using method of the full-automatic pretreatment color titration analyzer. The automatic titration device is mainly used for realizing the purpose of automatic titration, can greatly reduce manual participation, has stable experimental flow and environment in the titration process, eliminates unnecessary interference and improves the accuracy of detection results.
Description
Technical Field
The invention relates to the technical field of titration analysis, in particular to a full-automatic pretreatment color titration analyzer, and in addition, the invention also relates to a using method of the full-automatic pretreatment color titration analyzer.
Background
Titration refers to a quantitative analysis means and is also a chemical experimental operation. It determines the content of a solute by performing a specific pretreatment such as high temperature digestion reflux and then allowing quantitative reactions of two or more solutions. The method is characterized in that the titration end point is indicated according to the color change of an indicator, then the consumption volume of a standard solution is visually detected, and the analysis result is calculated to determine the exact content of the analyzed substance.
Digestion, also known as wet digestion, is a method of destroying organic or reducing substances in a sample with an acid or alkali solution and under heating. The usual acidolysis systems are: nitric acid-sulfuric acid, nitric acid-perchloric acid, hydrofluoric acid, hydrogen peroxide, etc., which can totally destroy organic and reducing substances such as cyanide, nitrite, sulfide, sulfite, thiosulfate, and thermally unstable substances such as thiocyanate, etc., in sewage and sediment; caustic soda solution is commonly used for alkaline hydrolysis. Digestion may be carried out in a crucible (nickel or polytetrafluoroethylene), or a high-pressure digestion tank may be used. The problems to be noted in digestion are: (1) the components to be measured cannot be lost in the digestion process; (2) the introduction of interfering substances is not necessary; (3) the method is safe and quick, and does not bring difficulty to the subsequent operation steps; (4) the digested solution must be suitable for the chosen monitoring method.
The calibration mainly comprises a direct calibration mode and an indirect calibration mode, wherein the direct calibration mode comprises the following steps of: accurately weighing a certain amount of reference substance, dissolving in water, and titrating with a solution to be calibrated until the reaction is complete. According to the consumed volume of the solution to be calibrated and the quality of the reference substance, calculating the accurate concentration of the solution to be calibrated; and (3) indirect calibration: there is a portion of the standard solution that is not suitable for calibration, but can only be calibrated with another standard solution of known concentration. If the acetic acid solution is calibrated by NaOH standard solution, the oxalic acid solution is calibrated by KMnO4 standard solution, and the like, the system error of indirect calibration is larger than that of direct calibration.
Because the manual titration process is complicated, an experimenter needs to sample, dilute, prepare samples, digest, transfer reagents, titrate, calculate results, write reports and other works, the workload is large, the steps are complicated, the consumed time is long, the quality of operators is unstable, and unexpected deviation can be caused to the titration results. Moreover, the existing titration apparatuses in the market do not meet the national standard, the automation degree is low, the effect is single, and the manual work cannot be completely liberated. Therefore, in order to better implement titration, a new type of automatic titration apparatus is needed.
Disclosure of Invention
The invention aims to provide a full-automatic pretreatment color titration analyzer which is mainly used for realizing the purpose of automatic titration, can greatly reduce the participation of manpower, has stable experimental flow and environment in the titration process, eliminates unnecessary interference and improves the accuracy of detection results.
In order to solve the technical problems, the invention adopts the following technical scheme:
a full-automatic pretreatment color titration analyzer comprises a base and a bracket arranged on the base, wherein a titration cup placement position and a digestion tube mounting frame are arranged on the bracket, and a temperature-controllable heating device is arranged below the digestion tube mounting frame;
the system comprises a support, a liquid path flow system, a control system and a detection system, wherein the liquid path flow system, the control system and the detection system are arranged on the support, the liquid path flow system and the detection system are connected with the control system, and the detection system is used for controlling the circulation of reagents in the liquid path flow system and realizing the titration of the reagents in a titration cup at the position where the titration cup is placed;
the liquid path system comprises a first diaphragm pump, a first switch electromagnetic valve, a first three-way switching valve and a second diaphragm pump which are sequentially connected from left to right; the first three-way switching valve is connected with the COM gear of the first multi-way switching valve through a first quantitative ring, one gear of the first multi-way switching valve is used for being connected with the titration cup, the other gear is connected with the COM gear of the second multi-way switching valve through a second three-way switching valve, and the other gears are used for being connected with samples, reagents and pure water; one gear of the second multi-way switching valve is a waste liquid end, and the rest gears are used for corresponding to digestion pipes on the digestion pipe mounting frame; the second three-way switching valve is connected with the titration cup through a third diaphragm pump;
the liquid path system also comprises a fourth multi-way switching valve, a fourth diaphragm pump, a third multi-way switching valve, a first precise injection pump, a second precise injection pump, a peristaltic pump, a third three-way switching valve, a fifth diaphragm pump, a second switch electromagnetic valve and a sixth diaphragm pump;
the COM gear of the fourth multi-way switching valve is connected with the COM gear of the third multi-way switching valve through a fourth diaphragm pump and a second quantitative ring, other gears of the fourth multi-way switching valve are used for connecting pure water, air and reagents, one gear of the third multi-way switching valve is a waste liquid end, and the other gears are used for corresponding to the digestion pipe;
the peristaltic pump, the sixth diaphragm pump, the first precise injection pump and the second precise injection pump are all used for being connected with the titration cup;
the COM gear of the third three-way switching valve is connected with the titration cup through the fifth diaphragm pump and the second switching electromagnetic valve, and the ON gear and the OFF gear of the third three-way switching valve are respectively used for being connected with high-concentration waste liquid and low-concentration waste liquid.
In one embodiment of the present disclosure, peristaltic pumps are used in conjunction with the reagents.
In one embodiment of the present disclosure, a sixth diaphragm pump is used in connection with pure water.
In one embodiment of the present disclosure, first and second precision syringe pumps are used in conjunction with the reagents.
In one embodiment of the present disclosure, a reagent rack for placing reagent bottles is arranged at the top of the bracket.
In one embodiment of the invention, the control system comprises a PCB mounting frame arranged on a bracket, an MCU micro-control unit control board arranged on the PCB mounting frame and a HUB multiport transponder connected with the MCU micro-control unit control board, wherein the HUB multiport transponder is connected with a terminal and a peristaltic pump driver, upper computer software is arranged in the terminal, and the peristaltic pump is connected with the peristaltic pump driver; the MCU micro-control unit control board is connected with a power supply control board and a switching power supply, and the temperature-controllable heating device is connected with the MCU micro-control unit control board;
the system comprises a first multi-way switching valve, a second multi-way switching valve, a third multi-way switching valve, a fourth multi-way switching valve, a first precise injection pump, a second precise injection pump and a detection system, wherein the detection system is connected with the HUB multi-port transponder;
the first, second, third, fourth, fifth and sixth diaphragm pumps, the first, second switch electromagnetic valves, the first, second and third three-way switching valves are connected with MCU micro-control unit control panel.
In one embodiment of the invention, a cooling fan is arranged on the bracket and is connected with the MCU control board through the speed regulation control board.
In one embodiment of the invention, a magnetic stirrer is arranged below the titration cup placement position and is connected with the MCU micro-control unit control board through the speed regulation control board.
In addition, the invention also discloses a using method of the full-automatic pretreatment color titration analyzer, which specifically comprises the following steps:
step 1: sample adding;
step 2: adding a reagent;
step 3: carrying out digestion reaction on the liquid in the digestion tube;
step 4: transferring the digested liquid into a titration cup;
step 5: titration is carried out;
step 6: calibrating;
step 7: cleaning the digestion tube;
step 8: cleaning a titration cup;
step 9: the upper computer software judges the titration end point according to the color change, calculates the concentration of titration liquid drops according to calibration, calculates the concentration of the measured substance and automatically reports.
Compared with the prior art, the invention has the following beneficial effects:
the invention mainly comprises a base, a bracket, a liquid path flow path system, a control system and a detection system, and in actual use, the invention is designed in a full-flow automatic way, thereby greatly reducing the participation of staff; the testing process has stable environment and strict experimental flow, unnecessary interference is eliminated, and the obtained detection result is more stable and accurate; meanwhile, the quantitative ring is adopted for quantification, so that the cost is saved, and the popularization is convenient; more importantly, the invention has no moving structures such as mechanical arms and the like, has low failure rate and is convenient for maintenance.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of the present invention.
Fig. 2 is a rear view of fig. 1 of the present invention.
Fig. 3 is an overall view of the liquid path system of the present invention.
FIG. 4 is a schematic view of portion A of FIG. 3 in accordance with the present invention.
FIG. 5 is a schematic view of portion B of FIG. 3 according to the present invention.
FIG. 6 is a schematic view of portion C of FIG. 3 in accordance with the present invention.
FIG. 7 is a schematic view of portion D of FIG. 3 according to the present invention.
Fig. 8 is a schematic diagram and connection relationship between the components of the present invention.
FIG. 9 is a schematic view of portion I of FIG. 8 in accordance with the present invention.
FIG. 10 is a schematic view of portion II of FIG. 8 in accordance with the present invention.
Reference numerals:
1-first diaphragm pump, 2-first switch solenoid valve, 3-first three-way switching valve, 4-second diaphragm pump, 5-first multi-way switching valve, 6-second three-way switching valve, 7-third diaphragm pump, 8-second multi-way switching valve, 9-third multi-way switching valve, 10-fourth diaphragm pump, 11-fourth multi-way switching valve, 12-first precision syringe pump, 13-second precision syringe pump, 14-peristaltic pump, 15-second switch solenoid valve, 16-fifth diaphragm pump, 17-third three-way switching valve, 18-sixth diaphragm pump, the device comprises a titration cup, a 20-background lamp, a 21-color identification module, a 22-magnetic stirrer, a 23-magnetic stirrer, a 24-digestion tube, a 25-controllable temperature heating device, a 26-first quantitative ring, a 27-second quantitative ring, a 28-MCU micro-control unit control board, a 29-peristaltic pump driver, a 30-HUB multiport transponder, a 31-speed regulation control board, a 32-power control board, a 33-power switch, a 34-cooling fan, a 35-digestion tube mounting frame, a 36-base, a 37-reagent frame, a 38-desktop computer and 39-upper computer software.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in numerous different ways without departing from the spirit or scope of the embodiments of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
In the description of the embodiments of the present invention, it should be understood that the terms "length," "vertical," "horizontal," "top," "bottom," and the like indicate an orientation or a positional relationship based on that shown in the drawings, and are merely for convenience in describing the embodiments of the present invention and to simplify the description, rather than to indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the embodiments of the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the embodiments of the present invention, the meaning of "plurality" is two or more, unless explicitly defined otherwise.
In the embodiments of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured" and the like are to be construed broadly and include, for example, either permanently connected, removably connected, or integrally formed; the device can be mechanically connected, electrically connected and communicated; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the embodiments of the present invention will be understood by those of ordinary skill in the art according to specific circumstances.
In embodiments of the invention, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, or may include both the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is less level than the second feature.
The following disclosure provides many different implementations, or examples, for implementing different configurations of embodiments of the invention. In order to simplify the disclosure of embodiments of the present invention, components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit embodiments of the present invention. Furthermore, embodiments of the present invention may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Referring to fig. 1-10, the embodiment discloses a full-automatic pretreatment color titration analyzer, which comprises a base 36 and a bracket arranged on the base 36, wherein a titration cup placement position and a digestion tube mounting frame 35 are arranged on the bracket, and a controllable temperature heating device 25 is arranged below the digestion tube mounting frame 35;
the device also comprises a liquid path flow path system, a control system and a detection system which are arranged on the bracket, wherein the liquid path flow path system and the detection system are connected with the control system, and the detection system is used for controlling the circulation of the reagent in the liquid path flow path system and realizing the titration of the reagent in the titration cup 19 at the placement position of the titration cup;
the liquid path system comprises a first diaphragm pump 1, a first switching electromagnetic valve 2, a first three-way switching valve 3 and a second diaphragm pump 4 which are connected together in sequence from left to right; the first three-way switching valve 3 is connected with the COM gear of the first multi-way switching valve 5 through a first quantitative ring 26, one gear of the first multi-way switching valve 5 is used for being connected with the titration cup 19, the other gear is connected with the COM gear of the second multi-way switching valve 8 through a second three-way switching valve 6, and the other gears are used for connecting samples, reagents and pure water; one gear of the second multi-way switching valve 8 is a waste liquid end, and the rest gears are used for corresponding to the digestion tubes 24 on the digestion tube mounting frame; the second three-way switching valve 6 is connected with the titration cup 19 through a third diaphragm pump 7;
the liquid path flow system further comprises a fourth multi-way switching valve 11, a fourth diaphragm pump 10, a third multi-way switching valve 9, a first precise injection pump 12, a second precise injection pump 13, a peristaltic pump 14, a third three-way switching valve 17, a fifth diaphragm pump 16, a second on-off electromagnetic valve 15 and a sixth diaphragm pump 18;
the COM gear of the fourth multi-way switching valve 11 is connected with the COM gear of the third multi-way switching valve 9 through the fourth diaphragm pump 10 and the second quantifying ring 27, the rest gears of the fourth multi-way switching valve 11 are used for connecting pure water, air and reagent, one gear of the third multi-way switching valve 9 is a waste liquid end, and the rest gears are used for corresponding to the digestion pipe 24;
peristaltic pump 14, sixth diaphragm pump 18, first, second precision syringe pumps are all used to connect with titration cup 19;
the COM gear of the third three-way switching valve 17 is connected to the titration cup 19 through the fifth diaphragm pump 16 and the second switching solenoid valve 15, and the third three-way switching valve 17 ON and the OFF gear are respectively connected to the high-concentration waste liquid and the low-concentration waste liquid.
In this embodiment, it should be noted that, an end of the first diaphragm pump 1 far from the first switch electromagnetic valve 2 is a waste liquid end for discharging the waste liquid 1;
one end of the second diaphragm pump 4 far away from the first three-way switching valve 3 is an air end;
the first switch electromagnetic valve 2 is connected with the ON gear of the first three-way switching valve 3; the second diaphragm pump 4 is connected to the OFF range of the first three-way switching valve 3.
In the present embodiment of the present invention, in the present embodiment,
the first multi-way switching valve 5 is an 8-gear switching valve, and the specific gear is as follows: S1-S8, wherein, pure water 1 is connected to S1 gear, sample is connected to S2 gear, reagent 3 is connected to S3 gear, reagent 4 is connected to S4 gear, S5 gear is used for being connected with titration cup 19, S6 gear is used for being connected with the ON gear of second three-way change-over valve 6, S7 gear is used for being connected with reagent 1, and S8 gear is used for being connected with reagent 2.
The second multi-way switching valve 8 is a 16-gear switching valve, and the S16 gear is used for discharging the waste liquid 2; the remaining gear positions are used to configure the digestion tube 24.
The third multi-way switching valve 9 is a 16-gear switching valve, and the S16 gear is used for discharging the reagent 3; the remainder are used to configure the digestion tube 24.
The fourth multi-way switching valve 11 is a 6-gear switching valve, the S1 gear is communicated with air, the S2 gear is used for being connected with pure water 2, the S3 gear is used for being connected with a reagent 5, the S4 gear is used for being connected with the reagent 6, and the S and S6 gears are in a blocking state to form a blocking position;
the first precise injection pump and the second precise injection pump are used for being connected with the reagent; the first precise injection pump 12 is connected with the reagent 7, and the second precise injection pump 13 is connected with the reagent 8; peristaltic pump 14 is connected to reagent 9 and sixth diaphragm pump 18 is connected to pure water.
The number of digestion tubes 24 may be configured according to actual requirements.
Further preferably, the top of the bracket is provided with a reagent rack 37 for placing reagent bottles.
The control system comprises a PCB mounting frame, an MCU micro control unit control board 28 and a HUB multiport repeater 30, wherein the PCB mounting frame is mounted on the support, the MCU micro control unit control board 28 is arranged on the PCB mounting frame, the HUB multiport repeater 30 is connected with a terminal and a peristaltic pump driver 29, upper computer software 39 is arranged in the terminal, and the peristaltic pump 14 is connected with the peristaltic pump driver 29; the MCU micro-control unit control board 28 is connected with a power supply control board 32 and a switching power supply, and the controllable temperature heating device 25 is connected with the MCU micro-control unit control board 28;
wherein, the first, second, third and fourth multi-way switching valves, the first and second precise injection pumps, the detection system is connected with the HUB multiport repeater 30;
the first, second, third, fourth, fifth and sixth diaphragm pumps, the first, second switch solenoid valves, the first, second and third three-way switching valves are connected with MCU micro-control unit control board 28.
Further preferably, a cooling fan 34 is arranged on the bracket, and the cooling fan 34 is connected with the MCU control board 28 through the speed regulation control board 31.
Wherein, be located titration cup and place the position below and be provided with magnetic stirrer 22, magnetic stirrer 22 passes through speed governing control panel 31 is connected with MCU micro-control unit control panel 28.
In this embodiment, the magnetic stirrer 22 is used to drive the magnetic stirrer 23 to rotate, so as to stir the liquid.
The detection system comprises a background light 20 and a color recognition module 21, and the background light 20 and the color recognition module 21 are connected with an MCU micro-control unit control board 28; a backlight 20 for titrating the illumination background, assisting the color recognition module 21 to work; the color recognition module 21 is used for color recognition in the titration process, and transmits real-time color data to the upper computer software 39 for analysis and processing.
For a further understanding of the present invention by those skilled in the art, the specific functions of the components are further defined as follows:
in this embodiment:
a first diaphragm pump 1 for withdrawing liquid from the digestion tube 24 and filling the first dosing ring 26;
a first on-off solenoid valve 2 for locking the liquid in the first dosing ring 26;
a first three-way switching valve 3 for switching a flow path and filling or emptying the first dosing ring 26;
a second diaphragm pump 4 for evacuating the liquid in the first dosing ring 26;
a first multi-way switching valve 5 for switching reagent and sample types;
a second three-way switching valve 6 for switching a flow path to a COM range of the second multi-way switching valve 8 or to a titration cup 19;
a third diaphragm pump 7 for pumping the liquid in the digestion tube 24 into the titration cup 19;
the second multi-way switching valve 8 is used for switching the pipe position and the waste liquid level of the digestion pipe 24;
a third multi-way switching valve 9 is used for switching the tube position and the waste liquid level of the digestion tube 24 and the titration cup 19.
And a fourth diaphragm pump 10 for pumping the liquid into the third multi-way switching valve 9COM range (port).
A fourth multi-way switching valve 11 for switching the kind of reagent and the air level;
a first precision syringe pump 12 for dripping the reagent 7 into the titration cup 19;
a second precision syringe pump 13 for dripping the reagent 8 into the titration cup 19;
a peristaltic pump 14 for adding reagent 9 to titration cup 19;
a second on-off solenoid valve 15 for locking the liquid in the titration cup 19 against siphoning;
a fifth diaphragm pump 16 for drawing the waste liquid from the titration cup 19;
the third three-way switching valve 17 is used for switching the flow directions of waste liquid with different concentrations in the titration cup 19;
a sixth diaphragm pump 18 for spraying pure water into the titration cup 19 for cleaning;
a titration cup 19, which is a reaction vessel for the reagent;
a backlight 20 for titrating the illumination background, assisting the color recognition module 21 to work;
the color recognition module 21 is used for recognizing the color in the titration process and transmitting real-time color data to the upper computer software 39;
a magnetic stirrer 22 for driving a magnetic stirrer 23 to rotate;
a magnetic stirrer 23 which rotates to stir the liquid;
digestion tube 24 for digestion reflux reaction of the reagents;
a temperature-controllable heating device 25 for temperature-controlled heating of the digestion tube 24;
a first dosing ring 26 for accurately dosing a liquid;
a second dosing ring 27 for accurately dosing the liquid;
a cooling fan 34 for cooling the digestion tube 24;
a digestion tube mounting frame 35 for fixing the digestion tube 24;
a base 36 for mounting the temperature controllable heating device 25 and other components;
a reagent rack 37 for placing reagent bottles;
the PCB mounting rack is used for mounting MCU micro-control unit control boards 28 and the like;
in actual use, the bracket is provided with a pump valve mounting plate for mounting components such as a pump, a valve and the like;
MCU micro control unit control board 28: is arranged on the PCB mounting frame and serves as a control core of all the switching power supplies and the temperature-controllable heating device 25.
A peristaltic pump drive 29 for driving the peristaltic pump 14 into motion;
HUB multiport transponder circuit board: the integrated circuit is arranged on the PCB mounting frame and used as an integration of the communication port;
a speed control plate 31 for speed control of the magnetic stirrer 22 and the cooling fan 34;
a power control board 32 for power control of the whole machine;
a power switch 33 for converting 220VAC current into 24VDC current;
in this embodiment, the terminal is a desktop computer 38: as the upper computer, an operator operates the upper computer software 39 through the upper computer; the upper computer software 39 includes a man-machine interface, a complete set of workflow control, an algorithm of the detection module, report issuing functions and the like, and will not be described in detail herein.
Example two
The embodiment discloses a method for using a full-automatic pretreatment color titration analyzer, which specifically comprises the following steps:
step 1: the sample is added in,
s1: the first multi-way switching valve 5 is switched to the sample position S2 to be connected with the COM gear, the first three-way switching valve 3 is switched to the ON gear to be connected with the COM gear, the first switching electromagnetic valve 2 is set to be in an open state, and the first diaphragm pump 1 is started until the sample liquid is filled in the first quantitative ring 26;
s2: after the sample is filled with the first metering ring 26, the first diaphragm pump 1 and the first switch electromagnetic valve 2 are closed, the first multi-way switching valve 5 to the S6 gear is switched to be connected with the ON gear of the second three-way electromagnetic valve, the second three-way electromagnetic valve is switched to be connected with the COM gear, and the second multi-way electromagnetic valve is switched to be connected with the corresponding digestion pipe 24, such as S1;
s3: the first three-way switching valve 3 is switched to the OFF gear and the COM gear, the second diaphragm pump 4 is opened, and the sample in the first quantitative ring 26 is discharged to the digestion tube 24 by air.
Step 2: adding a reagent;
s1, specifically comprising adding reagent 1-4,
s101, switching a first multi-way switching valve 5 to a reagent position to be connected with a COM gear, switching a first three-way switching valve 3 to an ON gear to be connected with the COM gear, setting a first switching electromagnetic valve 2 to be in an open state, and starting a first diaphragm pump 1 until sample liquid is filled in a first quantitative ring 26;
s102: after the sample is filled with the first metering ring 26, the first diaphragm pump 1 and the first switch electromagnetic valve 2 are closed, the first multi-way switching valve 5 to the S6 gear is switched to be connected with the ON gear of the second three-way electromagnetic valve, the second three-way electromagnetic valve is switched to be connected with the COM gear, and the second multi-way electromagnetic valve is switched to be connected with the corresponding digestion pipe 24, such as S1;
s102: the first three-way switching valve 3 is switched to the OFF gear and the COM gear, the second diaphragm pump 4 is opened, and the reagent in the first quantitative ring 26 is discharged into the digestion tube 24 by air.
S2: also comprises the addition of a reagent 5-6,
s201: the third multi-way switching valve 9 is switched to a COM gear and is connected with the waste liquid position, the fourth multi-way switching valve 11 is switched to a reagent position and is connected with the COM gear, and the fourth diaphragm pump 10 is opened to pump full reagent to the second quantitative ring 27;
s202: after full filling, the fourth diaphragm pump 10 is closed, the fourth multi-way switching valve 11 is switched to a dead blocking position (blocking position) of the S6 gear connected with the COM gear, the third multi-way switching valve 9 is switched to a digestion tube 24 position, for example S1, the fourth multi-way switching valve 11 is switched to an air position, and the fourth diaphragm pump 10 is opened to discharge the reagent in the second quantitative ring 27 to the digestion tube 24 by air.
Step 3: performing digestion reaction on the liquid in the digestion tube 24;
the temperature-controllable heating device 25 is heated to a set temperature, the cooling fan 34 is started for condensation, and heating and digestion are carried out for a preset time.
Step 4: transferring the digested liquid to a titration cup 19;
the second multi-way switching valve 8 is switched to a digestion position, for example, the S1 gear is connected with the COM gear, the second three-way switching valve 6 is switched to the OFF gear to be connected with the COM gear, the third diaphragm pump 7 is opened, and all liquid in the digestion tube 24 is transferred to the titration cup 19.
Step 5: titration is carried out;
after the digested liquid is transferred to the titration cup 19, the magnetic stirrer 22 is turned on, the background light 20 is turned on, the peristaltic pump 14 is operated to add the reagent 9, the program automatically selects to drop the reagent into the titration cup 19 by using the first precise injection pump 12 or the second precise injection pump 13, the amount of the titration reagent consumed when the titration end point is judged by recording the color change, and the related data of the measured liquid is automatically calculated and reported.
Step 6: calibrating;
s1: the first multi-way switching valve 5 is switched to the calibration reagent position to be connected with the COM gear, the first three-way switching valve 3 is switched to the ON gear to be connected with the COM gear, the first switching electromagnetic valve 2 is set to be in an open state, and the first diaphragm pump 1 is started until the calibration reagent liquid is filled in the first metering ring 26.
S2: after the calibration reagent fills the first metering ring 26, the first diaphragm pump 1 and the first switch electromagnetic valve 2 are closed, the first multi-way switching valve 5 is switched to the S6 gear position to be connected with the ON gear position of the second three-way electromagnetic valve, the second three-way electromagnetic valve is switched to the ON gear position to be connected with the COM gear position, and the second multi-way electromagnetic valve is switched to the titration cup 19 position, such as the S5 gear position;
s3: switching the first three-way switching valve 3 to the OFF gear and the COM gear, opening the second diaphragm pump 4, and discharging the labeled reagent from the first quantifying ring 26 to the titration cup 19 by using air;
s4: the third multi-way switching valve 9 is switched to a COM gear and is connected with the waste liquid phase, the fourth multi-way switching valve 11 is switched to a calibration reagent position and is connected with a COM unit, and the fourth diaphragm pump 10 is opened to pump full reagent to the second quantitative ring 27;
s5: after the filling, the fourth diaphragm pump 10 is closed, the fourth multi-way switching valve 11 is switched to a dead blocking position, which is connected with the COM gear, of the S6 gear, and the third multi-way switching valve 9 is switched to a titration cup 19 position, such as S15;
s6: switching the fourth multi-way switching valve 11 to an air gear, opening the fourth diaphragm pump 10, and discharging the calibration reagent in the second quantifying ring 27 to the titration cup 19 by using air;
s7: the magnetic stirrer 22 is turned on, the background light 20 is turned on, the peristaltic pump 14 is operated to add the reagent 9, the upper computer software 39 automatically selects to drop the reagent into the titration cup 19 by using the first precise injection pump 12 or the second precise injection pump 13, the amount of the titration reagent consumed when the titration end point is judged by recording the color change, and the related data of the calibrated reagent is automatically calculated and reported.
Step 7: cleaning the digestion tube 24;
s1: the second multi-way switching valve 8 is switched to a corresponding digestion pipe 24 position, for example, an S1 gear is connected with a COM gear, the second three-way switching valve 6 is switched to an ON gear and a COM gear, the first multi-way switching valve 5 is switched to an S6 gear and a COM gear, the first three-way switching valve 3 is switched to an ON gear and a COM gear, the first switching electromagnetic valve 2 is opened, the first diaphragm pump 1 is opened, and liquid in the digestion pipe 24 is pumped out;
s2: the third multi-way switching valve 9 is switched to a digestion tube 24, for example, an S1 gear is connected with a COM gear, the fourth multi-way switching valve 11 is switched to a pure water position, for example, an S2 gear, the fourth diaphragm pump 10 is opened to spray pure water into the corresponding digestion tube 24, the fourth diaphragm pump 10 is closed after reaching a preset time, and the first diaphragm pump 1 is closed after the liquid in the digestion tube 24 is emptied.
Step 8: cleaning the titration cup 19;
according to the waste liquid concentration of the titration cup 19, the upper computer software 39 automatically selects and switches the third three-way switching valve 17 to the COM gear to connect with the ON gear or the OFF gear, the second switch electromagnetic valve 15 is opened, the fifth diaphragm pump 16 is opened to pump out the waste liquid in the titration cup 19, the sixth diaphragm pump 18 is opened to spray pure water into the titration cup 19, the sixth diaphragm pump 18 is closed after the circulation is repeated for a plurality of times, the fifth diaphragm pump 16 is closed after the liquid in the titration cup 19 is discharged, and the second switch electromagnetic valve 15 is closed.
Step 9: the upper computer software 39 judges the titration end point according to the color change, calculates the concentration of the titration liquid drop according to the calibration, calculates the concentration of the measured substance and automatically reports.
According to the invention, automatic titration and cleaning are realized by arranging the liquid path system, and meanwhile, the accuracy of titration can be effectively improved by adopting color recognition as an endpoint judgment mode of titration; meanwhile, the reagent and the sample can be accurately quantified by filling or emptying the quantifying ring, so that the titration accuracy is further improved; and the condensate reflux is achieved by the provision of the heat radiation fan 34.
The reagents used in the test are all analytical reagents meeting the national standard, and the experimental water is newly prepared ultrapure water, distilled water or water with the same purity
In practical use, the invention has the following advantages:
1. the invention realizes full process automation, comprises functions of dilution, sampling, sample preparation, digestion, transfer, titration, cleaning, calculating results, reporting and the like, and saves time and labor cost by one-key operation;
2. judging a titration end point by adopting color, and completely conforming to the experimental flow of a national standard method;
3. the reagent sample is accurately quantified by adopting the quantifying ring, so that the quantifying volume is accurate, the repeatability is good, the speed is high, the efficiency is high, and the cost is saved;
4. the flow is stable, the accuracy of experimental results is high, the repeatability is good, the interference is avoided, and the interference of personnel and other factors is reduced;
5. the digestion temperature is uniform and controllable, the cooling reflux efficiency is high, and the structure is simple;
6. high and low concentration is titrated simultaneously, so that the purpose of full-automatic switching is realized;
7. and the mechanical arm and other moving structures are not needed, and the maintenance is more convenient.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
The foregoing description of the preferred embodiment of the invention is not intended to be limiting, but rather to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The full-automatic pretreatment color titration analyzer is characterized by comprising a base and a bracket arranged on the base, wherein a titration cup placement position and a digestion tube mounting frame are arranged on the bracket, and a temperature-controllable heating device is arranged below the digestion tube mounting frame;
the system comprises a support, a liquid path flow system, a control system and a detection system, wherein the liquid path flow system, the control system and the detection system are arranged on the support, the liquid path flow system and the detection system are connected with the control system, and the detection system is used for controlling the circulation of reagents in the liquid path flow system and realizing the titration of the reagents in a titration cup at the position where the titration cup is placed;
the liquid path system comprises a first diaphragm pump, a first switch electromagnetic valve, a first three-way switching valve and a second diaphragm pump which are sequentially connected from left to right; the first three-way switching valve is connected with the COM gear of the first multi-way switching valve through a first quantitative ring, one gear of the first multi-way switching valve is used for being connected with the titration cup, the other gear is connected with the COM gear of the second multi-way switching valve through a second three-way switching valve, and the other gears are used for being connected with samples, reagents and pure water; one gear of the second multi-way switching valve is a waste liquid end, and the rest gears are used for corresponding to digestion pipes on the digestion pipe mounting frame; the second three-way switching valve is connected with the titration cup through a third diaphragm pump;
the liquid path system also comprises a fourth multi-way switching valve, a fourth diaphragm pump, a third multi-way switching valve, a first precise injection pump, a second precise injection pump, a peristaltic pump, a third three-way switching valve, a fifth diaphragm pump, a second switch electromagnetic valve and a sixth diaphragm pump;
the COM gear of the fourth multi-way switching valve is connected with the COM gear of the third multi-way switching valve through a fourth diaphragm pump and a second quantitative ring, other gears of the fourth multi-way switching valve are used for connecting pure water, air and reagents, one gear of the third multi-way switching valve is a waste liquid end, and the other gears are used for corresponding to the digestion pipe;
the peristaltic pump, the sixth diaphragm pump, the first precise injection pump and the second precise injection pump are all used for being connected with the titration cup;
the COM gear of the third three-way switching valve is connected with the titration cup through the fifth diaphragm pump and the second switching electromagnetic valve, and the ON gear and the OFF gear of the third three-way switching valve are respectively used for being connected with high-concentration waste liquid and low-concentration waste liquid.
2. A fully automated pretreatment color titration analyzer as recited in claim 1, wherein: peristaltic pumps are used in conjunction with the reagents.
3. A fully automated pretreatment color titration analyzer as recited in claim 1, wherein: the sixth diaphragm pump is used for being connected with pure water.
4. A fully automated pretreatment color titration analyzer as recited in claim 1, wherein: the first and second precision injection pumps are used for connecting with the reagent.
5. A fully automated pretreatment color titration analyzer as recited in claim 1, wherein: the top of the bracket is provided with a reagent rack for placing reagent bottles.
6. A fully automated pretreatment color titration analyzer as recited in claim 1, wherein: the control system comprises a PCB mounting frame arranged on the bracket, an MCU micro-control unit control board arranged on the PCB mounting frame and a HUB multi-port transponder connected with the MCU micro-control unit control board, wherein the HUB multi-port transponder is connected with a terminal and a peristaltic pump driver, upper computer software is arranged in the terminal, and the peristaltic pump is connected with the peristaltic pump driver; the MCU micro-control unit control board is connected with a power supply control board and a switching power supply, and the temperature-controllable heating device is connected with the MCU micro-control unit control board;
the system comprises a first multi-way switching valve, a second multi-way switching valve, a third multi-way switching valve, a fourth multi-way switching valve, a first precise injection pump, a second precise injection pump and a detection system, wherein the detection system is connected with the HUB multi-port transponder;
the first, second, third, fourth, fifth and sixth diaphragm pumps, the first, second switch electromagnetic valves, the first, second and third three-way switching valves are connected with MCU micro-control unit control panel.
7. A fully automated pretreatment color titration analyzer as recited in claim 6, wherein: and a cooling fan is arranged on the bracket and is connected with the MCU control panel through the speed regulation control panel.
8. A fully automated pretreatment color titration analyzer as recited in claim 7, wherein: the magnetic stirrer is arranged below the titration cup placement position and is connected with the MCU micro-control unit control board through the speed regulation control board.
9. A method of using a fully automated pretreatment color titration analyzer according to any of claims 1-8, comprising the steps of:
step 1: sample adding;
step 2: adding a reagent;
step 3: carrying out digestion reaction on the liquid in the digestion tube;
step 4: transferring the digested liquid into a titration cup;
step 5: titration is carried out;
step 6: calibrating;
step 7: cleaning the digestion tube;
step 8: cleaning a titration cup;
step 9: the upper computer software judges the titration end point according to the color change, calculates the concentration of titration liquid drops according to calibration, calculates the concentration of the measured substance and automatically reports.
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