CN111487116A - Pneumatic solution dilution distribution calibration method - Google Patents
Pneumatic solution dilution distribution calibration method Download PDFInfo
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- CN111487116A CN111487116A CN202010224163.3A CN202010224163A CN111487116A CN 111487116 A CN111487116 A CN 111487116A CN 202010224163 A CN202010224163 A CN 202010224163A CN 111487116 A CN111487116 A CN 111487116A
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- 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
- G01N1/38—Diluting, dispersing or mixing samples
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- 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
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- 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
- G01N2001/2893—Preparing calibration standards
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Abstract
The invention discloses a pneumatic type solution dilution distribution calibration method, which comprises the steps of putting pure water into a solution standard substance bottle A, emptying a diluent bottle B, putting a waste liquid bottle G on a weighing balance, electrifying an electromagnetic valve I CT1 and an electromagnetic valve III CT3, recording the first index of the weighing balance at the moment, electrifying an electromagnetic valve II CT2 and an electromagnetic valve seven CT7, recording the second index of the weighing balance at the moment, and obtaining the calibrated volume of a quantitative tube according to the first index and the second index.
Description
Technical Field
The invention relates to a calibration method for solution dilution distribution, and belongs to the technical field of solution preparation.
Background
In the detection work of the water quality on-line analyzer (instrument), a detector generally adopts a water quality solution standard substance to detect and maintain the instrument. The stability of the standard substance of the low-concentration water solution is poor, the detection standard generally needs detection personnel to dilute the standard substance of the high-concentration solution, the on-site preparation of the low-concentration solution is carried out manually in an experiment, the on-site environment of the water quality on-line analyzer is complex, the preparation condition cannot meet the standard requirement, the preparation amount of the low-concentration solution is large, the manual preparation working steps are complex, the time and the labor are consumed, and the accuracy of the amount value of the diluted solution is difficult to guarantee. Therefore, a technology capable of automatically diluting a solution under a complex environment with high dilution accuracy under the complex environment is urgently needed.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a pneumatic solution dilution distribution calibration method, and the volume calibrated by the method is used, so that the concentration accuracy of the obtained diluted standard solution is high.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:
a pneumatic solution dilution dispensing calibration method comprising the steps of:
calibration of the volume of the dosing tube C in the pressure controller degree p, ambient temperature T:
step 1.1), recording pressure reading p and ambient temperature T of a pressure controller, putting pure water into a solution standard substance bottle A, emptying a diluent bottle B, and putting a waste liquid bottle G on a weighing balance;
step 1.2), electrifying the solenoid valve I CT1 and the solenoid valve III CT3, opening a normally closed outlet of the solenoid valve I CT1 and a normally closed inlet of the solenoid valve III CT3, introducing nitrogen into the solution standard substance bottle A through the normally closed outlet of the solenoid valve I CT1, pressing out pure water from the solution standard substance bottle A through pressure, and passing the pure water through the solution standard substance bottle AA normally closed inlet of the electromagnetic valve three CT3 enters the quantitative pipe C; keeping the starting state, ensuring that the quantitative tube C is full, and enabling the redundant liquid to flow into a waste liquid bottle G through a normally open outlet of the electromagnetic valve four-CT 4; then the first electromagnetic valve CT1 and the third electromagnetic valve CT3 are powered off, and the quantitative pipe C is filled with pure water; record the reading m of the weighing balance at this time1-0；
Step 1.3), electrifying an electromagnetic valve II CT2 and an electromagnetic valve seven CT7, opening a normally closed outlet of an electromagnetic valve II CT2 and a normally closed outlet of an electromagnetic valve seven CT7 at the moment, feeding nitrogen into a diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, feeding the nitrogen into a normally open inlet of an electromagnetic valve III CT3 through the normally open outlet of the electromagnetic valve seven CT7 by passing through the normally open inlet of the electromagnetic valve III CT3, and keeping the electromagnetic valve II CT2 and the electromagnetic valve seven CT7 electrified for a period of time to ensure that a quantitative ring is emptied by the nitrogen, and allowing pure water to flow into a waste liquid bottle G through the normally open outlet of an electromagnetic valve IV CT 4; record the reading m of the weighing balance at this time1-1(ii) a Then, closing the second electromagnetic valve CT2 and the seventh electromagnetic valve CT7, and at the moment, the quantitative tube C is in an emptying state;
step 1.4), calculating:
in the formula (I), the compound is shown in the specification,
the pressure controller measures the volume rho of the pipe C under the degree p and the ambient temperature TTThe density of the pure water is T at the ambient temperature;
step 1.5), counting; and repeating the steps 1.1) to 1.4) under different pressure controller pressure readings p and environment temperatures T to obtain the volumes of the quantitative pipes C under different pressure controller pressure readings p and environment temperatures T.
Preferably: calibration of the volume of the volumetric flask D:
step 2.1), weighing and recording the weight m of the empty bottle of the target solution storage bottle I at the specific temperature of 20 DEG C2-0Pure water is filled in the diluent bottle B;
step 2.2), electrifying the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve IV CT7, opening a normally closed outlet of the electromagnetic valve II CT2, a normally closed outlet of the electromagnetic valve IV CT4 and a normally closed outlet of the electromagnetic valve IV CT7, enabling nitrogen to enter a diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, pressing out pure water through pressure, entering a normally open inlet of the electromagnetic valve III CT3 through the normally open outlet of the electromagnetic valve IV CT7, entering a quantitative tube C through the normally open inlet of the electromagnetic valve III CT3, entering the electromagnetic valve IV CT4 through the quantitative tube C, entering an inlet tube I F through the normally closed outlet of the electromagnetic valve IV CT4, injecting the pure water into a constant volume bottle D, keeping for a period of time, and completing constant volume work after the liquid level rises and is detected by the ultrasonic locator H; closing a second solenoid valve CT2, a fourth solenoid valve CT4 and a seventh solenoid valve CT 7; at the moment, the electromagnetic valve is switched to a liquid discharging state, the electromagnetic valve five CT5 and the electromagnetic valve six CT6 are opened, nitrogen enters a normally closed inlet of the electromagnetic valve five CT5 through a normally open outlet of the electromagnetic valve two CT2 at the moment, enters the constant volume bottle D through the electromagnetic valve five CT5, the interior of the bottle is in a positive pressure state, pure water in the constant volume bottle D enters the target liquid storage bottle I through a normally closed inlet of the electromagnetic valve six CT6, the target liquid storage bottle I is taken down, and data m is recorded by weighing2-1；
Step 2.3), calculating:
wherein, V2Is the volume of a constant volume bottle D, rho2The density of water at a particular temperature.
Preferably: the specific temperature range in step 2.1) is 10-30 ℃.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the volumes of the quantitative tube C and the quantitative bottle D are calibrated in different environments, and the accuracy of the concentration of the diluted standard solution is higher by using the calibrated volumes of the quantitative tube C and the quantitative bottle D.
Drawings
FIG. 1 is an electrical schematic of the present invention;
FIG. 2 is a schematic structural view of the present invention;
fig. 3 is a schematic view showing the structure of a sealed container bottle.
Detailed Description
The present invention is further illustrated by the following description in conjunction with the accompanying drawings and the specific embodiments, it is to be understood that these examples are given solely for the purpose of illustration and are not intended as a definition of the limits of the invention, since various equivalent modifications will occur to those skilled in the art upon reading the present invention and fall within the limits of the appended claims.
A pneumatic solution dilution and distribution device is shown in figures 1 and 2 and comprises a touch display, a circuit control module, a first electromagnetic valve CT1, a second electromagnetic valve CT2, a third electromagnetic valve CT3, a fourth electromagnetic valve CT4, a fifth electromagnetic valve CT5, a sixth electromagnetic valve CT6, a seventh electromagnetic valve CT7, a solution standard substance bottle A, a diluent liquid bottle B, a quantifying pipe C, a constant volume bottle D, an ultrasonic positioner H, a target solution storage bottle I, a waste liquid bottle G, an auxiliary nitrogen bottle GP and a pressure controller WYF, wherein the touch display, the first electromagnetic valve CT1, the second electromagnetic valve CT2, the third electromagnetic valve CT3, the fourth electromagnetic valve CT4, the fifth electromagnetic valve CT5, the sixth electromagnetic valve CT6, the seventh electromagnetic valve CT7, the ultrasonic positioner H and the pressure controller WYF are all connected with the circuit control module. In this embodiment, the first solenoid valve CT1, the second solenoid valve CT2, the third solenoid valve CT3, the fourth solenoid valve CT4, the fifth solenoid valve CT5, the sixth solenoid valve CT6 and the seventh solenoid valve CT7 are two-position three-way solenoid valves, in another embodiment of the present invention, the first solenoid valve CT1, the fifth solenoid valve CT5, the sixth solenoid valve CT6 and the seventh solenoid valve CT7 are through solenoid valves, and the second solenoid valve CT2, the third solenoid valve CT3 and the fourth solenoid valve CT4 are two-position three-way solenoid valves, wherein:
the auxiliary nitrogen cylinder GP is respectively connected with an inlet of the first electromagnetic valve CT1 and an inlet of the second electromagnetic valve CT2, and the pressure controller WYF is arranged on a circuit connecting the auxiliary nitrogen cylinder GP with the inlet of the first electromagnetic valve CT1 and the inlet of the second electromagnetic valve CT 2.
The normally closed outlet of the first electromagnetic valve CT1 is connected with the inlet of the first pipeline of the solution standard substance bottle A, the normally open outlet of the first electromagnetic valve CT1 is normally open, and the outlet of the second pipeline of the solution standard substance bottle A is connected with the normally closed inlet of the third electromagnetic valve CT 3. The first pipeline of the solution standard substance bottle A and the second pipeline of the solution standard substance bottle A both extend into the solution standard substance bottle A, and the outlet of the first pipeline of the solution standard substance bottle A is lower than the inlet of the second pipeline of the solution standard substance bottle A.
The normally closed outlet of the second electromagnetic valve CT2 is connected with the inlet of the first pipeline of the diluent bottle B, the normally open outlet of the second electromagnetic valve CT2 is connected with the normally closed inlet of the five electromagnetic valve CT5, the normally open inlet of the five electromagnetic valve CT5 is normally open, the outlet of the second pipeline of the diluent bottle B is connected with the inlet of the seven electromagnetic valve CT7, the normally closed outlet of the seven electromagnetic valve CT7 is connected with the normally open inlet of the three electromagnetic valve CT3, and the normally open outlet of the seven electromagnetic valve CT7 is normally open. The first pipeline of the diluent bottle B and the second pipeline of the diluent bottle B extend into the diluent bottle B, and the outlet of the first pipeline of the diluent bottle B is lower than the inlet of the second pipeline of the diluent bottle B.
The outlet of the electromagnetic valve three CT3 is connected with the inlet of the quantitative tube C, the outlet of the quantitative tube C is connected with the inlet of the electromagnetic valve four CT4, the normally open outlet of the electromagnetic valve four CT4 is connected with the waste liquid bottle G, and the normally closed outlet of the electromagnetic valve four CT4 is connected with the inlet tube I F of the constant volume bottle D. And the outlet of the solenoid valve five CT5 is connected with the inlet II E of the constant volume bottle D. The outlet of the constant-volume bottle D is connected with a normally closed inlet of a solenoid valve six CT6, a normally open inlet of a solenoid valve six CT6 is normally open, and the outlet of the solenoid valve six CT6 is connected with a target solution storage bottle I.
And the outlet of the outlet pipe of the solution standard substance bottle A. The first inlet pipe F extends into the constant volume bottle D, the ultrasonic positioner H is arranged on the constant volume bottle D, the ultrasonic positioner H is located between the outlet of the first inlet pipe F and the second inlet E of the constant volume bottle D, the outlet of the first inlet pipe F is lower than the ultrasonic sensor H, and the fluctuation of the liquid level is reduced to improve the positioning accuracy. The second inlet E is arranged on the side surface of the fixed-volume bottle D. The position of the pipeline in the constant volume bottle can reduce the liquid level shaking in the constant volume process, thereby being beneficial to the ultrasonic positioner to judge the work of the end point and achieving the purpose of improving the constant volume precision.
All parts of the device are connected by gas-liquid pipelines, the pipelines are made of PEEK, and the drift diameter is 2 mm. The whole device is protected by clean nitrogen in the dilution process, and the risk of environmental air pollution is avoided. The solution dilution and transfer work by using air pressure has the advantages of preparing the solution without contact and reducing external pollution in the solution preparation process.
The specifications of the two-position three-way electromagnetic valve (CT 1-CT 7) are as follows: the drift diameter is 2mm, the valve body is made of POM and PTEF, and the working pressure is-50 kPa-300 kPa.
As shown in fig. 3, the solution standard substance bottle a and the diluent bottle B are sealed container bottles, the bottle body is made of borosilicate, the bottle cap is made of PP, two connectors are fixed on the top opening of the bottle cap and connected with a gas-liquid dual-purpose pipeline, two pipelines are provided, namely a pipeline i and a pipeline ii, the pipeline i is a gas/liquid inlet pipe, the pipeline ii is a gas/liquid outlet pipe, and the outlet of the pipeline i is higher than the inlet of the pipeline ii, so that the gas entering the pipeline i can generate pressure in the bottle to press out the liquid in the bottle from the pipeline ii.
Quantitative bottle C is the peek material, and the latus rectum is 2 mm.
The fixed-volume bottle D is made of high borosilicate material, the wall thickness is 3mm, the shape is a small-diameter fat belly cone bottom, the outer diameter of the small-diameter part is 20mm, and the height is 200 mm. The width of the cone bottom part of the fat belly is 150mm, and the height is 100 mm. The lowest point of the cone bottom part is provided with a hole which is externally connected with a pipeline.
The top of the constant volume bottle is sealed, the distance between the ultrasonic positioner and the bottle mouth is 50mm, the 1 st pipeline (inlet pipe I) F at the top extends into the bottle through the interface, the distance between the pipeline mouth and the top of the constant volume bottle is 150mm, and the 2 nd pipeline at the top is connected to the side surface E interface.
The constant volume bottle has the sealing property, ensures that no environmental air pollution risk exists in the constant volume process, reduces the volatilization effect of liquid and improves the constant volume precision.
A pneumatic solution dilution dispensing method comprising the steps of:
step 1, preparing: the detector puts the standard substance into the bottle A and puts the diluent into the bottle B.
Step 2, starting up: the tester starting device, solenoid valve one CT1, solenoid valve two CT2, solenoid valve three CT3, solenoid valve four CT4, solenoid valve five CT5, solenoid valve six CT6, solenoid valve seven CT7 all are in normal open position at this moment, namely not electrified, solenoid valve internal line is connected with NC (electrified)/NO (deenergized) two kinds of states, solenoid valve state is shown as table 1 at this moment: and opening a GP valve of the auxiliary nitrogen cylinder, and controlling the nitrogen pressure to be 0.15MPa by the pressure controller WYF. Inputting the concentration information of the standard substance in the solution, the adding times n of the quantitative tube C and the reading information of the pressure controller.
TABLE 1 solenoid valve status in step 2
| Valve number | CT1 | CT2 | CT3 | CT4 | CT5 | CT6 | CT7 |
| Status of state | NO | NO | NO | NO | NO | NO | NO |
Step 3, filling a quantitative ring with a solution standard substance: and energizing the first solenoid valve CT1 and the third solenoid valve CT3, wherein the states of the solenoid valves are shown in Table 2, and when the solenoid valves are in the starting state, the normally closed outlet of the first solenoid valve CT1 and the normally closed inlet of the third solenoid valve CT3 are opened, nitrogen enters the solution standard substance bottle A through the normally closed outlet of the first solenoid valve CT1, the solution standard substance is pressed out of the solution standard substance bottle A through pressure, and enters the quantitative tube C through the normally closed inlet of the third solenoid valve CT 3. And the first solenoid valve CT1 and the third solenoid valve CT3 are kept electrified for 3s, in another embodiment of the invention, the first solenoid valve CT1 and the third solenoid valve CT3 are kept electrified for 1s, in yet another embodiment of the invention, the first solenoid valve CT1 and the third solenoid valve CT3 are kept electrified for 5s, the quantitative tube C is fully filled, and the redundant liquid flows into the waste liquid cup G through a normally-open outlet of the fourth solenoid valve CT 4. Then the solenoid valve one CT1 and the solenoid valve three CT3 are powered off, the solenoid valves are in the ending state, and the quantitative tube C is filled with the static solution standard substance.
TABLE 2 solenoid valve status in step 3
Step 4, filling a quantitative ring with diluent: the solenoid valve II CT2 and the solenoid valve seven CT7 are electrified, the states of the solenoid valves are shown in the table 3, when the device is in the starting state, the normally closed outlet of the electromagnetic valve II CT2 and the normally closed outlet of the electromagnetic valve seven CT7 are opened, nitrogen enters the diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, the diluent is pressed out by pressure and enters a normally open inlet of a solenoid valve three CT3 through a normally open outlet of a solenoid valve seven CT7, the liquid enters the quantitative tube C through a normally open inlet of the electromagnetic valve three CT3, the electromagnetic valve two CT2 and the electromagnetic valve seven CT7 are kept electrified for 5s, in another embodiment of the present invention, solenoid two CT2 and solenoid seven CT7 are kept energized for 3s, in yet another embodiment of the present invention, the solenoid valve two CT2 and the solenoid valve seven CT7 are kept energized for 7s to ensure that the dosing ring is filled with diluent, and the excess liquid flows into the waste liquid cup G through the normally open outlet of the solenoid valve four CT 4. Thereafter, the second solenoid valve CT2 and the seventh solenoid valve CT7 are closed, and the solenoid valves are in the closed state, and the fixed amount tube C is filled with the stationary diluent.
TABLE 3 solenoid valve status in step 4
And 5, filling the quantitative ring with the solution standard substance, and repeating the step 3.
Step 6, quantitative ring injection: energizing a second electromagnetic valve CT2, a fourth electromagnetic valve CT4 and a seventh electromagnetic valve CT7, wherein the state of the electromagnetic valves is as shown in Table 4, when the electromagnetic valves are in a starting state, a normally closed outlet of the second electromagnetic valve CT2, a normally closed outlet of the fourth electromagnetic valve CT4 and a normally closed outlet of the seventh electromagnetic valve CT7 are opened, nitrogen enters a diluent bottle B through the normally closed outlet of the second electromagnetic valve CT2, diluent is pressed out through pressure, enters a normally open inlet of the third electromagnetic valve CT3 through a normally open outlet of the seventh electromagnetic valve CT7, enters a dosing tube C through a normally open inlet of the third electromagnetic valve CT3, original solution standard substances in the dosing tube C are pressed out, enters an inlet tube F through a normally closed outlet of the fourth electromagnetic valve CT4 and is injected into a solenoid valve D, the energization 5s of the second electromagnetic valve CT2, the fourth electromagnetic valve CT4 and the seventh electromagnetic valve CT7 are kept energized, and in another embodiment of the invention, the energization 5s of the second, The electromagnetic valve seven CT7 is electrified for 3s, in yet another embodiment of the invention, the electromagnetic valve two CT2, the electromagnetic valve four CT4 and the electromagnetic valve seven CT7 are electrified for 7s, so that the solution standard substance in the quantifying pipe C is completely transferred to the holding bottle D, and then the electromagnetic valve two CT2, the electromagnetic valve four CT4 and the electromagnetic valve seven CT7 are closed, so that the electromagnetic valve is in an end state. And repeating the steps 5 and 6 for n times according to the adding times n of the quantitative tubes.
TABLE 4 solenoid valve status in step 6
Step 7, sample preparation: the solenoid valve two CT2, the solenoid valve four CT4 and the solenoid valve seven CT7 are electrified, the states of the solenoid valves are shown in the table 5, when the device is in the starting state, the normally closed outlet of the electromagnetic valve II CT2, the normally closed outlet of the electromagnetic valve IV CT4 and the normally closed outlet of the electromagnetic valve seven CT7 are opened, nitrogen enters the diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, the diluent is pressed out by pressure and enters a normally open inlet of a solenoid valve three CT3 through a normally open outlet of a solenoid valve seven CT7, enters the quantitative tube C through a normally open inlet of the electromagnetic valve three CT3, enters the electromagnetic valve four CT4 through the quantitative tube C, the liquid enters an inlet pipe I F through a normally closed outlet of an electromagnetic valve four CT4 and is injected into a constant volume bottle D, the constant volume bottle D is kept for a period of time until the liquid level rises, and after the liquid level is detected by the ultrasonic positioner H, the constant volume operation is completed, and the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve VII CT7 are closed. At the moment, the electromagnetic valve is switched to a liquid discharging state, the electromagnetic valve five CT5 and the electromagnetic valve six CT6 are opened, nitrogen enters a normally closed inlet of the electromagnetic valve five CT5 through a normally open outlet of the electromagnetic valve two CT2 and enters the constant volume bottle D through the electromagnetic valve five CT5, the interior of the bottle is in a positive pressure state, and solution in the constant volume bottle D enters the target liquid storage bottle I through a normally closed inlet of the electromagnetic valve six CT 6. The five solenoid valve CT5 and the six solenoid valve CT6 are closed, and the solenoid valves are in the end state.
TABLE 5 solenoid valve status in step 7
The concentration c of the diluted standard solution stored in the target solution storage bottle I is as follows:
wherein c is the concentration of the diluted standard solution, V1To quantify the volume of the tube C, V2For the volume of the fixed-volume bottle, n is the number of times the fixed-volume tube is added, p is the pressure reading of the pressure controller, T is the ambient temperature, c0Is the concentration of the standard substance of the solution,
the volume of tube C is quantified in degrees p of the pressure controller and at ambient temperature T.
Step 8, cleaning the cleaning fixed-volume bottle D:
and 81, disconnecting the target solution storage bottle I from the outlet of the solenoid valve five CT5, and connecting the outlet of the solenoid valve five CT5 to the waste liquid bottle G.
And 82, electrifying the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve IV CT7, opening a normally closed outlet of the electromagnetic valve II CT2, a normally closed outlet of the electromagnetic valve IV CT4 and a normally closed outlet of the electromagnetic valve IV CT7, enabling nitrogen to enter a diluent bottle B through a normally closed outlet of the electromagnetic valve II CT2, pressing out diluent through pressure, enabling the diluent to enter a normally open inlet of the electromagnetic valve III CT3 through a normally open outlet of the electromagnetic valve IV CT7, enabling the diluent to enter a quantifying pipe C through a normally open inlet of the electromagnetic valve III CT3, enabling the diluent to enter the electromagnetic valve IV CT4 through the quantifying pipe C, enabling the diluent to enter an inlet pipe F through a normally closed outlet of the electromagnetic valve IV CT4 and inject the diluent into a constant volume bottle D, keeping for a period of time, closing the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve IV CT 7. At the moment, the electromagnetic valve is switched to a liquid discharging state, the electromagnetic valve five CT5 and the electromagnetic valve six CT6 are opened, nitrogen enters a normally closed inlet of the electromagnetic valve five CT5 through a normally open outlet of the electromagnetic valve two CT2 and enters the constant volume bottle D through the electromagnetic valve five CT5, the interior of the bottle is in a positive pressure state, and solution in the constant volume bottle D enters the waste liquid bottle G through a normally closed inlet of the electromagnetic valve six CT 6.
And step 83, repeating the step 82 for more than three times to finish the cleaning of the fixed-volume bottle D.
A pneumatic solution dilution dispensing calibration method comprising the following steps.
For the volume of the quantitative tube C under the temperature T of the environment and the degree p of the pressure controller
Calibration of (2):
step 1.1), recording pressure reading p and ambient temperature T of a pressure controller by a detector, putting pure water into a solution standard substance bottle A, emptying a diluent bottle B, and putting a waste liquid bottle G on a weighing balance.
Step 1.2), electrifying the first solenoid valve CT1 and the third solenoid valve CT3, wherein the state of the solenoid valves is as shown in table 2, and when the solenoid valves are in the starting state, the normally closed outlet of the first solenoid valve CT1 and the normally closed inlet of the third solenoid valve CT3 are opened, nitrogen passes through the first solenoid valve CT3The normally closed outlet of the CT1 enters the solution standard substance bottle A, pure water is pressed out of the solution standard substance bottle A by pressure, and the pure water enters the quantitative tube C through the normally closed inlet of the electromagnetic valve three CT 3. Keeping the first solenoid valve CT1 and the third solenoid valve CT3 energized for 3s, keeping the first solenoid valve CT1 and the third solenoid valve CT3 energized for 1s in another embodiment of the invention, keeping the first solenoid valve CT1 and the third solenoid valve CT3 energized for 5s in yet another embodiment of the invention, ensuring that the quantitative tube C is full, and the redundant liquid flows into the waste liquid bottle G through a normally open outlet of the fourth solenoid valve CT 4. Then, the solenoid valve one CT1 and the solenoid valve three CT3 are powered off, and the quantitative pipe C is filled with pure water. Record the reading m of the weighing balance at this time1-0。
Step 1.3), electrifying the second solenoid valve CT2 and the seventh solenoid valve CT7, wherein the states of the solenoid valves are shown in Table 3, when the device is in the starting state, the normally closed outlet of the electromagnetic valve II CT2 and the normally closed outlet of the electromagnetic valve seven CT7 are opened, nitrogen enters the diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, the nitrogen passes through the diluent bottle B, enters a normally open inlet of a solenoid valve three CT3 through a normally open outlet of a solenoid valve seven CT7, finally enters a dosing pipe C through a normally open inlet of a solenoid valve three CT3, keeps the solenoid valve two CT2 and the solenoid valve seven CT7 electrified for 5s, in another embodiment of the present invention, solenoid two CT2 and solenoid seven CT7 are kept energized for 3s, in yet another embodiment of the present invention, the solenoid valve two CT2 and the solenoid valve seven CT7 are kept energized for 7s to ensure that the dosing ring is evacuated by nitrogen, and pure water flows into the waste liquid bottle G through the normally open outlet of the solenoid valve four CT 4. Record the reading m of the weighing balance at this time1-1. Thereafter, the second solenoid valve CT2 and the seventh solenoid valve CT7 are closed, and the metering tube C is in an empty state.
Step 1.4), calculating:
in the formula (I), the compound is shown in the specification,
the pressure controller measures the volume rho of the pipe C under the degree p and the ambient temperature TTIs at ambient temperatureThe density of pure water at T.
Step 1.5), counting. And repeating the steps 1.1) to 1.4) under different pressure controller pressure readings p and environment temperatures T to obtain the volumes of the quantitative pipes C under different pressure controller pressure readings p and environment temperatures T. And the pressure reading p range of the pressure controller is 0.12-0.18 MPa, the ambient temperature T range is 15-25 ℃, the obtained volumes of the quantitative tubes C under different pressure readings p and ambient temperatures T of the pressure controller are tabulated or are made into a fitting curve and are stored in the circuit control module, and when the device is used, the volumes of the quantitative tubes C under the given pressure reading p and the given ambient temperature T are obtained according to the prepared table or the fitting curve.
Volume V of constant volume bottle D2Calibration of (2):
step 2.1), weighing and recording the weight m of an empty bottle I of a target solution storage bottle by a detector under the condition that the ambient temperature is 20 DEG C2-0And pure water is filled in the diluent bottle B.
Step 2.2), electrifying the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve IV CT7, wherein the states of the electromagnetic valves are shown in table 5, when the electromagnetic valves are in the starting state, at the moment, the normally closed outlet of the electromagnetic valve II CT2, the normally closed outlet of the electromagnetic valve IV CT4 and the normally closed outlet of the electromagnetic valve IV CT7 are opened, nitrogen enters the diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, pure water is pressed out through pressure, the nitrogen enters the normally open inlet of the electromagnetic valve III CT3 through the normally open outlet of the electromagnetic valve IV CT7, the nitrogen enters the dosing pipe C through the normally open inlet of the electromagnetic valve III CT3, the nitrogen enters the electromagnetic valve IV CT4 through the dosing pipe C, the nitrogen enters the inlet pipe F through the normally closed outlet of the electromagnetic valve IV CT4 and is injected into the constant volume bottle D, the constant volume bottle D is kept for a period. Closing a solenoid valve two CT2, a solenoid valve four CT4 and a solenoid valve seven CT 7. At the moment, the electromagnetic valve is switched to a liquid discharging state, the electromagnetic valve five CT5 and the electromagnetic valve six CT6 are opened, nitrogen enters a normally closed inlet of the electromagnetic valve five CT5 through a normally open outlet of the electromagnetic valve two CT2 at the moment, enters the constant volume bottle D through the electromagnetic valve five CT5 and is in a positive pressure state, pure water in the constant volume bottle D enters the target liquid storage bottle I through a normally closed inlet of the electromagnetic valve six CT6, and a target is taken downLiquid storage bottle I and weighing recording data m2-1。
Step 2.3), calculating:
wherein, V2Is the volume of a constant volume bottle D, rho20Is the density of water at 20 ℃.
According to the invention, the volumes of the quantitative tube C and the volumetric flask D are calibrated, and the concentration accuracy of the diluted standard solution is higher by using the calibrated volumes of the quantitative tube C and the volumetric flask D.
The invention adopts a pneumatic type non-contact constant volume and liquid discharge mode, avoids the pollution to the solution and improves the preparation precision of the solution.
The invention can automatically dilute the solution standard substance and realize the on-site preparation and use of the low-concentration solution standard substance with large preparation quantity. The diluted solution has high value accuracy and traceability, and can be directly used for the field calibration work of the water quality on-line analyzer.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (3)
1. A pneumatic solution dilution dispensing calibration method, comprising the steps of:
calibration of the volume of the dosing tube C in the pressure controller degree p, ambient temperature T:
step 1.1), recording pressure reading p and ambient temperature T of a pressure controller, putting pure water into a solution standard substance bottle A, emptying a diluent bottle B, and putting a waste liquid bottle G on a weighing balance;
step 1.2), electrifying the first solenoid valve CT1 and the third solenoid valve CT3, wherein the normally closed outlet of the first solenoid valve CT1 and the normally closed inlet of the third solenoid valve CT3 are opened, and nitrogen passes through the first solenoid valve CT1The normally closed outlet enters a solution standard substance bottle A, pure water is pressed out of the solution standard substance bottle A through pressure, and enters a quantitative pipe C through a normally closed inlet of an electromagnetic valve three CT 3; keeping the starting state, ensuring that the quantitative tube C is full, and enabling the redundant liquid to flow into a waste liquid bottle G through a normally open outlet of the electromagnetic valve four-CT 4; then the first electromagnetic valve CT1 and the third electromagnetic valve CT3 are powered off, and the quantitative pipe C is filled with pure water; record the reading m of the weighing balance at this time1-0；
Step 1.3), electrifying an electromagnetic valve II CT2 and an electromagnetic valve seven CT7, opening a normally closed outlet of an electromagnetic valve II CT2 and a normally closed outlet of an electromagnetic valve seven CT7 at the moment, feeding nitrogen into a diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, feeding the nitrogen into a normally open inlet of an electromagnetic valve III CT3 through the normally open outlet of the electromagnetic valve seven CT7 by passing through the normally open inlet of the electromagnetic valve III CT3, and keeping the electromagnetic valve II CT2 and the electromagnetic valve seven CT7 electrified for a period of time to ensure that a quantitative ring is emptied by the nitrogen, and allowing pure water to flow into a waste liquid bottle G through the normally open outlet of an electromagnetic valve IV CT 4; record the reading m of the weighing balance at this time1-1(ii) a Then, closing the second electromagnetic valve CT2 and the seventh electromagnetic valve CT7, and at the moment, the quantitative tube C is in an emptying state;
step 1.4), calculating:
in the formula, V1 p,TThe pressure controller measures the volume rho of the pipe C under the degree p and the ambient temperature TTThe density of the pure water is T at the ambient temperature;
step 1.5), counting; and repeating the steps 1.1) to 1.4) under different pressure controller pressure readings p and environment temperatures T to obtain the volumes of the quantitative pipes C under different pressure controller pressure readings p and environment temperatures T.
2. Pneumatic solution dilution dispensing calibration method according to claim 1, characterized in that: calibration of the volume of the volumetric flask D:
step 2.1), under the condition of a specific temperature of 20 ℃,weighing and recording the weight m of the empty bottle I of the target solution storage bottle2-0Pure water is filled in the diluent bottle B;
step 2.2), electrifying the electromagnetic valve II CT2, the electromagnetic valve IV CT4 and the electromagnetic valve IV CT7, opening a normally closed outlet of the electromagnetic valve II CT2, a normally closed outlet of the electromagnetic valve IV CT4 and a normally closed outlet of the electromagnetic valve IV CT7, enabling nitrogen to enter a diluent bottle B through the normally closed outlet of the electromagnetic valve II CT2, pressing out pure water through pressure, entering a normally open inlet of the electromagnetic valve III CT3 through the normally open outlet of the electromagnetic valve IV CT7, entering a quantitative tube C through the normally open inlet of the electromagnetic valve III CT3, entering the electromagnetic valve IV CT4 through the quantitative tube C, entering an inlet tube I F through the normally closed outlet of the electromagnetic valve IV CT4, injecting the pure water into a constant volume bottle D, keeping for a period of time, and completing constant volume work after the liquid level rises and is detected by the ultrasonic locator H; closing a second solenoid valve CT2, a fourth solenoid valve CT4 and a seventh solenoid valve CT 7; at the moment, the electromagnetic valve is switched to a liquid discharging state, the electromagnetic valve five CT5 and the electromagnetic valve six CT6 are opened, nitrogen enters a normally closed inlet of the electromagnetic valve five CT5 through a normally open outlet of the electromagnetic valve two CT2 at the moment, enters the constant volume bottle D through the electromagnetic valve five CT5, the interior of the bottle is in a positive pressure state, pure water in the constant volume bottle D enters the target liquid storage bottle I through a normally closed inlet of the electromagnetic valve six CT6, the target liquid storage bottle I is taken down, and data m is recorded by weighing2-1；
Step 2.3), calculating:
wherein, V2Is the volume of a constant volume bottle D, rho2The density of water at a particular temperature.
3. Pneumatic solution dilution dispensing calibration method according to claim 2, characterized in that: the specific temperature range in step 2.1) is 10-30 ℃.
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| CN114636456A (en) * | 2022-05-18 | 2022-06-17 | 江苏省计量科学研究院(江苏省能源计量数据中心) | Quantitative ring volume calibration system and method |
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