Multi-flow-path pretreatment system for online titrator

Abstract

The invention discloses a multi-flow-path pretreatment system for an online titrator, and relates to the technical field of chemical analysis devices, the multi-flow-path pretreatment system comprises a metering unit, an acidification digestion unit, a liquid adding unit, a digestion auxiliary positioning unit and a cleaning unit; the acidification digestion unit comprises a digestion container, the digestion container is provided with an acid adding interface, a titrator connecting port, a cleaning interface and a water sample interface, and a liquid absorption piece is arranged in the digestion container and is communicated with the titrator connecting port through a telescopic pipe. The telescopic pipe and the heating unit are designed in a matched mode, the telescopic pipe adopts a child-mother pipe design, on one hand, movement of the liquid suction part can be achieved through self-telescopic matching, and on the other hand, the telescopic pipe and the heating unit can be made of different materials to be matched with the external heating unit for heating; according to the design, the internal structure of the digestion container is simplified to the greatest extent, and the pretreatment of heating digestion is facilitated.

Description

Technical Field

[0001] The invention relates to the technical field of chemical analysis devices, and in particular to a multi-flow path pretreatment system for an online titrator. Background Art

[0002] During the use of online titrators, various liquid samples will be encountered. Some samples need to be digested, acidified or adjusted in pH before titration, and some samples with a lot of suspended matter need to be homogenized. Therefore, due to the complexity of pre-treatment, the use of online titrators is limited and the applicability is reduced, which has a certain impact on the promotion of online titrators. In the determination and analysis of titration in the laboratory, the operation process needs to be completed manually step by step, such as heating digestion, adding solvent digestion, positioning and extracting the supernatant layer, etc. The workload is large and it is easy to cause human errors and affect the measurement results. Therefore, improving the work efficiency of titration analysis and the accuracy of measurement results, and realizing environmental protection, automation, and online detection are the current development trends. Summary of the invention

[0003] The purpose of the present invention is to solve the above-mentioned problem and to propose a multi-flow path pretreatment system for an online titrator.

[0004] In order to achieve the above object, the present invention adopts the following technical solutions:

[0005] A multi-flow path pretreatment system for an online titrator, comprising a metering unit, an acidification digestion unit, a liquid adding unit, a digestion auxiliary positioning unit, and a cleaning unit;

[0006] The acidification digestion unit comprises a digestion container, on which an acid addition interface, a titrator connection port, a cleaning interface, and a water sample interface are provided. The acid addition interface is connected to the acidification reagent container through a pipeline and a metering pump, the water sample interface is connected to the sample container through a pipeline and a metering pump, the cleaning interface is connected to a water source by a dual-channel peristaltic pump, and the titrator connection port is connected to the titrator;

[0007] A liquid absorbing component is arranged in the digestion container, and the liquid absorbing component is connected to the connection port of the titrator through a telescopic tube;

[0008] A cylinder is vertically mounted on the digestion container, and a piston rod of the cylinder is connected to the liquid absorbing component and drives the liquid absorbing component to move up and down.

[0009] Optionally, the telescopic tube is composed of two parts: a main tube and a sub-tube;

[0010] The main tube is made of heat-insulating ceramic material, the sub-tube is made of metal material, and a heating unit is arranged around the outer surface of the digestion container.

[0011] Optionally, the heating unit consists of two parts: a heat insulation material layer and an induction coil layer.

[0012] Optionally, the liquid absorbing member is composed of a fixing sleeve, a first fixing plate and a second fixing plate;

[0013] The fixing sleeve adopts an annular structure which is attached to the inner surface of the digestion container, the first fixing plate and the second fixing plate are symmetrically fixed on the upper and lower sides of the fixing sleeve, and the first fixing plate and the second fixing plate are both provided with liquid inlets connected to the outside.

[0014] Optionally, the first fixed plate is a semi-transparent mirror, and the second fixed plate is a total reflector with upper end reflection;

[0015] The outer surface of the digestion container is provided with a laser emitter, and the outer surface of the digestion container is provided with a transparent window for the laser to pass through;

[0016] The telescopic tube is provided with a laser receiver, and the inner surface of the telescopic tube is a smooth surface capable of reflecting light;

[0017] The laser transmitter and the laser receiver are both connected to the single-chip microcomputer. When the laser receiver does not receive the modulated laser from the laser transmitter, it outputs a low level and determines it as a muddy water layer. When it receives the modulated laser from the laser transmitter, it pulls down the corresponding pin level of the single-chip microcomputer and determines it as a clear water layer. When the electrical frequency changes frequently, it is determined to be the connecting layer between the clear water and muddy water layers.

[0018] Optionally, the liquid inlet is arranged at a blind spot of the laser receiver; and the cylinder is arranged on a side away from the laser transmitter.

[0019] Compared with the prior art, the present invention has the following advantages:

[0020] The present invention adopts a telescopic tube and a heating unit in a coordinated design. The telescopic tube adopts a mother-and-child tube design. On the one hand, the movement of the liquid-absorbing component can be realized through its own telescopic coordination. On the other hand, the two can be made of different materials and can be coordinated with an external heating unit for heating. Such a design simplifies the internal structure of the digestion container to the greatest extent, which is beneficial to the pretreatment of heating digestion.

[0021] The present invention adopts a laser positioning design. Through the cooperation of a laser transmitter, a liquid suction piece, a telescopic tube and a laser receiver, at least three auxiliary positioning functions can be realized on the basis of simplifying the internal structure of the digestion container to the greatest extent, which is beneficial to positioning after precipitation and convenient for the titrator to extract the supernatant.

[0022] The outstanding feature of the present invention is that it combines the functions of heating digestion, adding solvent for digestion, positioning and extracting the supernatant layer. On the one hand, the use of indirect physical means such as electromagnetic induction heating and laser can avoid adding parts in the digestion container to the greatest extent, resulting in the retention of solvent on the surface of the parts, which is inconvenient to clean and affects the purity of the solution. On the other hand, the use of laser capture can ensure that the moving liquid-absorbing parts can receive the laser in real time, so that real-time positioning can be performed, and at least three common solution forms such as the supernatant layer, the mixed layer and the connecting layer can be determined. The height of the connecting layer between the clear water and the turbid water layer can also be located and the height of the precipitation layer can be determined in combination with the size of the digestion container. The precipitation amount can be calculated to provide auxiliary parameters for the detection of the titrator. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a flow chart of the multi-flow path pretreatment system in the present invention;

[0024] Figure 2 It is a schematic diagram of the structure of the acidification digestion unit in the present invention (excluding the stirring unit);

[0025] Figure 3 It is a schematic diagram of the structure of the acidification digestion unit in the present invention (including the stirring unit);

[0026] Figure 4 This is a schematic diagram of the irradiation angle of the laser transmitter in the present invention;

[0027] Figure 5 This is a schematic diagram of the digestion auxiliary positioning unit in the present invention;

[0028] Figure 6 It is a schematic diagram of the telescopic tube structure in the present invention;

[0029] Figure 7 It is a schematic diagram of the structure of the liquid absorbing member in the present invention;

[0030] Figure 8 It is a schematic diagram of the heating unit structure in the present invention.

[0031] In the figure: 1 metering unit, 2 acidification digestion unit, 3 liquid adding unit, 4 digestion auxiliary positioning unit, 5 cleaning unit, 6 digestion container, 7 acid adding interface, 8 titrator connection port, 9 cleaning interface, 10 water sample interface, 11 metering pump, 12 dual-channel peristaltic pump, 13 laser receiver, 14 telescopic tube, 141 mother tube, 142 daughter tube, 15 liquid suction piece, 151 fixed sleeve, 152 first fixed plate, 153 second fixed plate, 154 liquid inlet, 16 laser transmitter, 17 heating unit, 171 thermal insulation material layer, 172 induction coil layer, 18 cylinder, 19 stirring bar, 20 magnetic stirrer. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0033] Embodiment 1

[0034] In high-sulfur wastewater, the wastewater is yellow and turbid because of the 1% hydrogen sulfide content. When the online titrator tests total iron and chloride, it affects the test endpoint judgment, resulting in the instrument not being able to analyze normally. With this system, extract 50mL of water sample and 150mL of 5% HNO3 solution at the same time, and heat and digest for 3-5 minutes at the same time. The solution can be decolorized and clarified, and then the analyzer extracts the clear liquid for accurate testing, and substitutes the dilution multiple in the calculation result.

[0035] The following is further described in detail through specific embodiments:

[0036] Reference Figure 1 , a multi-flow pretreatment system for an online titrator, comprising a metering unit 1, an acidification and digestion unit 2, a liquid addition unit 3, and a cleaning unit, and the process flow is as follows:

[0037] Step 1: The liquid sample is sent to the acidification and digestion unit 2 in a timed and quantitative manner through the metering unit 1. The acidification reagent is also quantitatively delivered to the acidification and digestion unit 2 by the metering unit 1 for acidification, heating, digestion and decolorization. During the digestion and decolorization process, the sample is fully stirred by the stirring unit, and then the peristaltic pump of the titrator (not shown in the figure) sucks the pretreated sample into the titrator (not shown in the figure) for analysis.

[0038] Step 2: The remaining sample in the acidification digestion unit 2 is pumped to the waste liquid recovery by the cleaning unit 5. The liquid adding unit 3 automatically adds water or solvent and repeats it 3 times to clean the acidification digestion tank. The waste liquid after cleaning is also pumped to the waste liquid recovery by the cleaning unit 5. During the cleaning process, the stirring unit stirs the whole process.

[0039] Reference Figure 2 and Figure 3 In this system, the acidification digestion unit 2 includes a digestion container 6, and the digestion container 6 is provided with an acid addition interface 7, a titrator connection port 8, a cleaning interface 9, and a water sample interface 10, as follows:

[0040] The acid addition interface 7 is connected to the acidification reagent container (not shown in the figure) through a pipeline and a metering pump 11, the water sample interface 10 is connected to the sample container (not shown in the figure) through a pipeline and a metering pump 11, the cleaning interface 9 is connected to the water source (not shown in the figure) by a dual-channel peristaltic pump 12, and the titrator connection port 8 is connected to the titrator (not shown in the figure).

[0041] Reference Figure 7, a liquid absorbing member 15 is provided in the digestion container 6. In this embodiment, the liquid absorbing member 15 is composed of a fixing sleeve 151, a first fixing plate 152 and a second fixing plate 153, and the specific connection method is as follows:

[0042] The fixing sleeve 151 is an annular structure that is in contact with the inner surface of the digestion container 6 , specifically an annular plate structure. Both sides of the fixing sleeve 151 may be in close contact with the inner surface of the digestion container 6 , or may be in contact with a gap.

[0043] The first fixing plate 152 and the second fixing plate 153 are symmetrically fixed on the upper and lower sides of the fixing sleeve 151. The first fixing plate 152 and the second fixing plate 153 are both provided with a liquid inlet 154 connected to the outside. The arrangement of the first fixing plate 152 and the second fixing plate 152 can form a liquid suction cavity. The liquid enters the liquid suction cavity through the liquid inlet 154, which is convenient for pumping liquid under the action of the negative pressure of the peristaltic pump of the titrator.

[0044] Reference Figure 3 and Figure 6 , the liquid-absorbing member 15 is connected to the titrator connection port 8 through the telescopic tube 14. The telescopic tube 14 is composed of a main tube 141 and a sub-tube 142, which are nested with each other. On the one hand, the movement of the liquid-absorbing member 15 can be realized through the telescopic cooperation of the main tube 141, and on the other hand, the two can be made of different materials, such as heat insulation and heating, as follows: the main tube 141 is made of heat-insulating ceramic material, the sub-tube 142 is made of metal material, and the outer surface of the digestion container 6 is surrounded by a heating unit 17, which is used to heat the metal material, and the heat-insulating ceramic material plays a role of heat insulation, so that directional heating can be achieved.

[0045] Reference Figure 8 The heating unit 17 is composed of two parts: a heat-insulating material layer 171 and an induction coil layer 172. A power source, such as a high-frequency power source, is connected to the induction coil layer 172, so that the sub-tube 142 made of metal material is directionally heated under the action of electromagnetic induction. The sub-tube 142 heats and digests the liquid in the digestion container 6 until the liquid is clarified.

[0046] Since the telescopic tube is a necessary component, electromagnetic induction heating is adopted. On the one hand, electromagnetic induction can be disassembled, and on the other hand, the structure in the digestion container 6 can be optimized to the greatest extent.

[0047] A cylinder 18 is vertically installed on the digestion container 6. The piston rod of the cylinder 18 is connected to the liquid absorption piece 15 and drives it to move up and down, so that it is convenient to move to the bottom to heat the liquid, and it is also convenient to locate the position where liquid needs to be extracted. For example, the liquid absorption piece 15 can be adjusted to move to a suitable position to only absorb the supernatant on the upper side.

[0048] Reference Figure 3In this embodiment, a stirring unit is also included, and the stirring unit is composed of a stirrer 19 and a magnetic stirrer 20. The bottom of the digestion container 6 should also be provided with a stirrer 19 and a magnetic stirrer 20. Figure 3 The stirring bar 19 adopts an elliptical structure, so that the liquid in the digestion container 6 can be magnetically stirred, and can also be rotated during cleaning to accelerate the movement of the fluid and make the cleaning more efficient.

[0049] Embodiment 2

[0050] The wastewater treatment device of the factory producing Freon needs to analyze COD and F-. However, since such wastewater is neutralized with lime, it contains a large amount of Ca(OH)2. During measurement, Ca(OH)2 will react with the reagent to form a precipitate, affecting the test and blocking the instrument pipeline. With this system, 50mL of water sample is extracted, and 150mL of 10% H2SO4 solution is extracted at the same time. After Ca(OH)2 and H2SO4 generate CaSO4 precipitate in the digestion container 6, let it stand for 2-3 minutes until the precipitate sinks, and then the analyzer extracts the upper clear liquid for accurate testing, and substitutes the dilution multiple into the calculation result.

[0051] Reference Figure 1 Compared with the first embodiment, this embodiment adds a digestion auxiliary positioning unit 4, which can be specifically divided into three parts: a transmitting end, a positioning end and a receiving end. The three parts will be described in detail below:

[0052] First, the transmitter (refer to Figure 2 , Figure 3 , Figure 4 and Figure 5 ), the outer surface of the digestion container 6 is provided with a laser emitter 16. In this embodiment, the laser emitter 16 should be tilted so that the emitted laser can point to the inner bottom end of the digestion container 6. The angle θ of the laser emitter 16 can also be adjusted by means of bolt tightening and loosening similar to the bracket adjustment, so that multi-angle laser can be achieved. In this embodiment, 30°≦θ≦60° can be flexibly selected according to the size of the digestion container 6. The outer surface of the digestion container 6 is provided with a transparent window for the laser to pass through. The laser emitter 16 emits a modulated laser of about 150KHz, and the laser passes through the transparent window to complete the emission operation. The advantage of the transmitting end is that: the positioning is performed by means of physical laser, which can avoid the use of structures and other means to increase the components inside the digestion container 6, avoid the problem of solvent retention in the components and the inconvenience of cleaning the outer surface, and also avoid the problem of corrosion of components and the problem that more mechanical components are prone to affect the purity of the solution.

[0053] Next is the positioning end (refer to Figure 4 , Figure 5 and Figure 7), the material of the first fixing plate 152 is changed to a semi-transparent mirror (half-reflecting mirror), and the material of the second fixing plate 153 is changed to a full-reflecting mirror for upper-end reflection. Such a configuration can give additional functions to the original parts without adding additional parts, and the semi-transparent mirror and the full-reflecting mirror cooperate with each other to reflect light, which is conducive to the determination of the positioning of the supernatant.

[0054] Finally, the receiving end (refer to Figure 4 and Figure 5 and Figure 6 ), a laser receiver 13 is arranged on the telescopic tube 14, and the inner surface of the telescopic tube 14 adopts a smooth surface that can reflect light, which can be a mirror surface of the metal material itself or a coating that can reflect light.

[0055] In this embodiment, the liquid inlet 154 is arranged at the blind spot of the laser receiver 13 (for example, within the 0-29° irradiation range of the laser emitter 16); the cylinder 18 is arranged on the side away from the laser emitter 16 (for example, above 61° of the irradiation range of the laser emitter 16) to avoid obstruction to positioning.

[0056] The laser transmitter 16 and the laser receiver 13 are both connected to a single-chip microcomputer, which can be a common STC 8051 single-chip microcomputer on the market, such as IAP15W413AS and other models.

[0057] The positioning principle of the digestion auxiliary positioning unit 4 is as follows: the modulated light of the laser transmitter 16 passes through the first fixed plate 152 of the semi-mirror, and then enters the telescopic tube 14 under the continuous reflection of the first fixed plate 151 (semi-mirror) and the second fixed plate 152 (total reflector), and is continuously reflected on its smooth surface (or reflective coating) like an optical fiber until it is captured by the laser receiver 16. The laser receiver 13 outputs a low level when it does not receive the modulated laser of the laser transmitter 16, and determines it as a muddy water layer; when it receives the modulated laser of the laser transmitter 16, it pulls down the corresponding pin level of the single-chip microcomputer and determines it as a clear water layer; when the electrical frequency changes frequently, it is determined to be a connecting layer between the clear water layer and the muddy water layer.

[0058] By setting up the digestion auxiliary positioning unit 4, this embodiment can, on the one hand, avoid another series of problems caused by adding parts in the digestion container 6 (see above) to the greatest extent; on the other hand, the laser capture method can ensure that the moving liquid-absorbing component 15 can receive the laser in real time, so that real-time positioning can be performed, and the above three common solution forms can be determined. For example, when Ca(OH)2 and H2SO4 generate CaSO4 precipitation, the supernatant layer can be located for extraction, and the height of the connecting layer between the clear water and the turbid water layer can be located and the height of the precipitation layer can be determined in combination with the size of the digestion container 6. The precipitation amount can be calculated to provide auxiliary parameters for the detection of the titrator.

[0059] The above description is only a preferred specific implementation mode of the present invention. It is impossible to list all the implementation modes here, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A multi-channel pretreatment system for an online titrator, characterized in that: It comprises a metering unit (1), an acidification and digestion unit (2), a liquid adding unit (3), a digestion auxiliary positioning unit (4), and a cleaning unit (5); The acidification digestion unit (2) comprises a digestion container (6), the digestion container (6) is provided with an acid addition interface (7), a titrator connection port (8), a cleaning interface (9), and a water sample interface (10), the acid addition interface (7) is connected to the acidification reagent container through a pipeline and a metering pump (11), the water sample interface (10) is connected to the sample container through a pipeline and a metering pump (11), the cleaning interface (9) has a dual-channel peristaltic pump (12) connected to a water source, and the titrator connection port (8) is connected to the titrator; A liquid absorbing component (15) is arranged in the digestion container (6), and the liquid absorbing component (15) is connected to the titrator connection port (8) via a telescopic tube (14); A cylinder (18) is vertically mounted on the digestion container (6), and a piston rod of the cylinder (18) is connected to the liquid absorbing member (15) to drive the liquid absorbing member to move up and down; The liquid absorbing member (15) is composed of a fixing sleeve (151), a first fixing plate (152) and a second fixing plate (153); The fixing sleeve (151) is an annular structure that is attached to the inner surface of the digestion container (6); the first fixing plate (152) and the second fixing plate (153) are symmetrically fixed on the upper and lower sides of the fixing sleeve (151); and the first fixing plate (152) and the second fixing plate (153) are both provided with a liquid inlet (154) that is connected to the outside; The first fixed plate (152) is a semi-transparent mirror, and the second fixed plate (153) is a total reflection mirror with upper end reflection; The outer surface of the digestion container (6) is provided with a laser emitter (16), and the outer surface of the digestion container (6) is provided with a transparent window for the laser to pass through; The telescopic tube (14) is provided with a laser receiver (13), and the inner surface of the telescopic tube (14) is a smooth surface capable of reflecting light. The laser transmitter (16) and the laser receiver (13) are both connected to the single chip microcomputer. When the laser receiver (13) does not receive the modulated laser from the laser transmitter (16), it outputs a low level and determines it as a muddy water layer. When it receives the modulated laser from the laser transmitter (16), it pulls down the level of the corresponding pin of the single chip microcomputer and determines it as a clear water layer. When the electrical frequency changes frequently, it is determined to be a connecting layer between the clear water layer and the muddy water layer. The telescopic tube (14) is composed of two parts: a main tube (141) and a sub-tube (142); The main tube (141) is made of heat-insulating ceramic material, the sub-tube (142) is made of metal material, and a heating unit (17) is arranged around the outer surface of the digestion container (6); The liquid inlet (154) is arranged at the blind spot of the laser receiver (13); and the cylinder (18) is arranged at a side away from the laser transmitter (16).

2. A multi-channel pretreatment system for an online titrator according to claim 1, characterized in that: The heating unit (17) is composed of two parts: a heat insulation material layer (171) and an induction coil layer (172).

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