CN214585054U

CN214585054U - Quantitative analysis device for trace urea

Info

Publication number: CN214585054U
Application number: CN202022852080.7U
Authority: CN
Inventors: 陈炜彧; 罗嘉豪; 周伟; 熊江磊; 李军冠; 张学良; 罗峥; 翟新桥
Original assignee: China Electronics System Engineering No2 Construction Co ltd
Current assignee: China Electronics System Engineering No2 Construction Co ltd
Priority date: 2020-12-02
Filing date: 2020-12-02
Publication date: 2021-11-02
Anticipated expiration: 2030-12-02

Abstract

The utility model relates to a water quality analysis technical field, concretely relates to trace urea quantitative analysis device aims at solving among the prior art and detects the precision limited, can't measure trace urea, and equipment advances kind automation and not high problem that forms of integration degree, and its technical essential lies in: including preprocessing device and detection device, preprocessing device with be provided with the microsample injector between the detection device, preprocessing device is used for handling the macromolecule organic matter, detection device includes connecting tube, reagent injection apparatus and conductivity cell, wherein connecting tube one end with the microsample injector intercommunication, one end is provided with the flow-through cell in addition for receive the water sample that detects the completion, reagent injection apparatus sets up the connecting tube is directional microsample injector one end, the conductivity cell sets up the connecting tube is directional flow-through cell one end. The trace urea quantitative analysis device has the advantages of high accuracy, high precision, good integration performance and the like.

Description

Quantitative analysis device for trace urea

Technical Field

The utility model relates to a water quality analysis technical field, concretely relates to trace urea quantitative analysis device.

Background

The ultrapure water is an essential auxiliary material for the production of products in semiconductor/liquid crystal panel factories, and the water quality requirement is quite high. Raw water for preparing ultrapure water is basically from municipal tap water, and the ultrapure water is obtained through multi-stage treatment of a pretreatment system, a preparation system and a polishing system and is used for product production in a semiconductor/liquid crystal panel factory.

Trace urea is sometimes doped into municipal tap water, the concentration is generally 50-200 PPb, and the conversion is only 10-40 PPb of TOC; the ultrapure water preparation system has limited urea removal capacity, and finally, the TOC of produced water exceeds the standard, the production yield is influenced, and huge economic loss is caused to a semiconductor/liquid crystal panel factory. When the existing ultrapure water system is designed, a urea removal unit is arranged at a raw water end, but the owner can reduce the operation cost and the actual operation time; and when the TOC of produced water exceeds the standard, the urea removal unit is started, and the method still brings certain economic loss. Even if a TOC instrument is arranged at the raw water end, trace urea cannot be doped to cause huge fluctuation of TOC; if the on-line monitoring of the trace urea is available, the urea removal unit is operated in time, so that economic loss can be avoided.

The prior art provides a spectrophotometric measuring method for urea detection technology, and the method has the disadvantages of large used part volume, low equipment integration degree, complicated sample introduction, long detection period up to more than 52min, poor practicability and no accordance with the continuous detection requirement of a pure water system. And the measurement precision is limited, and the trace urea cannot be measured.

SUMMERY OF THE UTILITY MODEL

Therefore, the to-be-solved technical problem of the utility model lies in overcoming among the prior art that it is limited to detect the precision, can't measure trace urea, and equipment advances kind automation and the not high defect that forms of integration degree to a trace urea quantitative analysis device is provided.

The above technical purpose of the present invention can be achieved by the following technical solutions:

the utility model provides a trace urea quantitative analysis device, includes preprocessing device and detection device, preprocessing device with be provided with the microsyringe between the detection device, preprocessing device is used for handling the macromolecule organic matter, detection device includes connecting tube, reagent injection apparatus and conductivity cell, wherein connecting tube one end with the microsyringe intercommunication, one end is provided with the circulation pond in addition for receive the water sample that detects the completion, reagent injection apparatus sets up the connecting tube is directional microsyringe one end, the conductivity cell sets up the connecting tube is directional circulation pond one end.

Preferably, preprocessing device includes inlet tube, water treatment component and drain pipe, the inlet tube with the water treatment component reaches the drain pipe communicates the setting respectively, the inlet tube is used for right the water treatment component carries out raw water and carries, the water treatment component is used for getting rid of the macromolecule organic matter in the raw water.

Preferably, the microsyringe is a six-way valve, one port of the microsyringe is connected with a water carrying unit, the rest part of the microsyringe is connected with the water treatment component, the drain pipe and the detection device, and the microsyringe is provided with an annular pipeline for mixing water carried in the water carrying unit with raw water in the pretreatment device and inputting the mixed water into the detection device.

Preferably, carry the water unit include with the water carrying pipeline that microsyringe intercommunication set up, water carrying pipeline keeps away from microsyringe one end with the setting is connected to the flow-through cell be provided with syringe pump, ion receiver and heating coil on the water carrying pipeline, the syringe pump sets up water carrying pipeline is directional microsyringe one end.

Preferably, the conductivity cells are provided in two, and a mixing coil is provided between the two conductivity cells.

Preferably, the water treatment component comprises an ultraviolet decomposer and an organic adsorber.

The application provides a trace urea quantitative analysis device, it injects oxidant combination solution into the connecting tube through reagent injection apparatus in, makes the effective and trace urea reaction of hydroxyl free radical that it produced, through the experiment, can accurately measure 20 ~ 1000 PPb's trace urea. And the sample to be measured keeps fluidity in the connecting pipeline, so that the sample to be measured is mentioned to a certain extent, the conditions such as residence time, reaction temperature, turbulence intensity and the like in the pipeline are the same, the repeatability of the measurement result is good, and the precision is high. Meanwhile, the pretreatment device, the microsyringe, the detection device, the water carrying unit and other components have high integration degree.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

Fig. 1 is a schematic structural diagram of a trace urea quantitative analysis device according to an embodiment of the present invention when the trace urea quantitative analysis device is in a loading gear.

Description of reference numerals:

1. a pretreatment device; 11. a water inlet pipe; 111. a first syringe pump; 112. a first flow sensor; 12. A water treatment assembly; 121. an ultraviolet decomposer; 122. an organic adsorber; 123. a service valve; 13. a drain pipe; 2. a microsyringe; 21. a port; 22. a loop circuit; 3. a water carrying unit; 31. a water carrying pipeline; 32. a second syringe pump; 33. a second flow sensor; 34. an ion receiver; 35. a heating coil; 4. A detection device; 41. a conductivity cell; 42. a reagent injection device; 43. a hybrid coil; 44. a drainage flow sensor; 45. the water pipe is communicated; 5. a flow-through cell.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Referring to fig. 1, a quantitative trace urea analyzer includes a pretreatment device 1, a micro-sampler 2, a water-carrying unit 3, a detection device 4, and a flow cell 5, where the pretreatment device 1 is used to pretreat raw water to remove impurities (such as macromolecular organic compounds) that may affect the determination of urea in the raw water, the micro-sampler 2 is respectively connected between the pretreatment device 1, the water-carrying unit 3, and the detection device 4, and is used to mix the raw water solution and the carried water and transmit the mixed water to the detection device 4 through a pipeline, and then detect the concentration of urea in the raw water through the detection device 4, and the flow cell 5 is used to collect the detected water flow.

Referring to fig. 1, the pretreatment device 1 includes a water inlet pipe 11, a water treatment assembly 12 and a water discharge pipe 13, the water inlet pipe 11 is respectively communicated with the water treatment assembly 12 and the water discharge pipe 13, in an embodiment, a pipeline leading to the water treatment assembly 12 and the water discharge pipe 13 is respectively disposed on the water inlet pipe 11, a first injection pump 111 and a first flow sensor 112 are disposed on the water inlet pipe 11, the first injection pump is used for pressurizing raw water in the water inlet pipe 11 to input raw water into the water treatment assembly 12, and the first flow sensor 112 is used for detecting a flow rate of the raw water to provide a signal of fluid in the water inlet pipe 11, so as to facilitate maintenance.

Referring to fig. 1, the water treatment module 12 includes an ultraviolet decomposer 121 and an organic adsorber 122, which are disposed in communication with each other, the ultraviolet decomposer 121 and the organic adsorber 122 are communicated with each other through a pipeline, a service valve 123 is disposed on the pipeline communicating between the ultraviolet decomposer 121 and the water inlet pipe 11, and the water treatment module 12 and the water outlet pipe 13 are communicated with each other through the micro-sampler 2. And (3) injecting raw water into the water treatment component 12 through the first injection pump 111 on the water inlet pipe 11 in the raw water conveying process, closing the maintenance valve 123 when the device needs maintenance, and discharging the raw water into the water discharge pipe 13 through a pipeline connecting the water inlet pipe 11 and the water discharge pipe 13. In an embodiment, the ultraviolet decomposer 121 is an ultraviolet lamp tube with a quartz sleeve arranged outside, and vacuum ultraviolet is used to remove macromolecular organic matters in raw water, wherein the wavelength range of the ultraviolet lamp tube is 100-200nm, specifically the wavelength range of the ultraviolet lamp tube is 180-190nm, and preferably the ultraviolet wavelength is 185 nm. The main body of the organic adsorber 122 is ion exchange resin, which uses macroporous strong base resin and macroporous weak base resin, the flow rate of raw water in the organic adsorber 122 is 1-2VB/h, and the ratio of water flow to resin is 2: 1-3: 1, wherein the organic adsorber 122 is used for adsorbing macromolecular organic matters, so as to improve the detection precision of the device, and the total organic carbon content of the raw water needs to be less than 2ppm to ensure that the pretreatment device 1 can effectively eliminate the influence of the macromolecular organic matters.

In one embodiment, the micro-sampler 2 is a six-way valve, referring to fig. 1, the micro-sampler 2 includes six ports 21 and an annular pipeline 22, the ports 21 are respectively labeled as i, ii, iii, iv, v, vi, wherein the annular pipeline 22 communicates the ports 21 ii and v with the port 21 v, the liquid flowing direction in the annular pipeline 22 is the ports 21 ii → 21 v, the ports 21 i communicate with the water treatment module 12, the ports 21 iii communicate with the water carrying unit 3, the ports 21 iv communicate with the detection device 4, and the unit vi communicates with the drain pipe 13. Referring to fig. 1, when the micro-sampler 2 is in the loading position, the raw water passes through the water treatment device, sequentially passes through the ports i, ii, v, and vi 21, and then flows out of the drain pipe 13 through the port vi 21, and when the micro-sampler 2 is in the sampling position, the raw water sequentially passes through the ports i and vi 21, and then flows out of the drain pipe 13 through the port vi 21. The water-carrying flow in the water-carrying unit 3 sequentially passes through the ports III, II, V and IV 21, is mixed with raw water in the annular pipeline 22 to form a sample to be detected, and is discharged into the detection device 4 through the port IV 21.

The water carrying unit 3 is configured to provide water carrying for a detection solution, the water carrying unit 3 includes a water carrying pipe 31 disposed in communication with the iii port 21, one end of the water carrying pipe 31 away from the iii port 21 is disposed in communication with the flow cell 5 to guide a water flow in the flow cell into the iii port 21, in an embodiment, the water carrying unit 3 further includes a second injection pump 32, a second flow sensor 33, an ion receiver 34, and a heating coil 35, wherein the second injection pump 32, the second flow sensor 33, the ion receiver 34, and the heating coil 35 are disposed in a direction from the flow cell 5 to the iii port 21 along the water carrying pipe 31, and the second injection pump 32 is configured to apply a pressure to the water flow in the flow cell 5 to make the water flow to the iii port 21. In one embodiment, the main body of the ion receiver 34 is ion exchange resin, which uses gel type strong acid resin and gel type strong base resin, and the flow rate of water is 40-60 VB/h, and the ratio is 3: 1. The heating coil 35 is used for keeping the temperature of the water carrying pipeline 31 at a suitable temperature, and in one embodiment, the temperature of the water carrying pipeline is 20-30 ℃, preferably 23-25 ℃.

Detection device 4 includes a plurality of conductivity cells 41, a plurality of reagent injection device 42, mixing coil 43, drainage flow sensor 44 and intercommunication water pipe 45, set up on the drainage flow sensor 44 on the intercommunication water pipe 45, a plurality of conductivity cell 41, a plurality of reagent injection device 42 and mixing coil 43 sets up and is connecting drainage flow sensor 44 reaches between the microsyringe 2. The reagent injection devices 42 are configured to inject a certain volume of reagent into the sample to be tested in the communication water pipe 45, in an embodiment, two reagent injection devices 42 are provided, the two reagent injection devices 42 are respectively configured to inject an alkaline reagent and an oxidant combined reagent, the reagent injection device 42 is respectively provided with a third injection pump 421 and a third flow sensor 422, and the third injection pump 421 and the third flow sensor 422 are communicated and provided on the communication water pipe 45 through a pipeline. In one embodiment, the alkaline agent may be a sodium hydroxide or potassium hydroxide solution with a concentration of 0.5 to 2%, preferably 1%. The oxidant combined reagent is a mixed solution of hypochlorite and bromide salt, preferably sodium salt, the concentration of the hypochlorite is 7-10 mM, the concentration of the bromide salt is 10-15 mM, and the molar ratio of the hypochlorite to the bromide salt is 0.6-0.7. The number of the conductivity cells 41 is two, the conductivity cells 41 are arranged between the reagent injection device 42 and the drainage flowmeter, a sample to be detected is injected with a reagent through the reagent injection device 42 and is mixed with the reagent, then the sample passes through the first conductivity cell 41, then passes through the mixing coil 43, and is promoted to react through the mixing coil 43, then passes through the conductivity cell 41 close to the drainage flowmeter, and finally is discharged into the flow cell 5 through a connecting pipeline, so that the detection of the urea concentration of the raw water is completed.

The working principle is as follows:

raw water is introduced through the first injection pump 111 on the water inlet pipe 11, so that the raw water enters the water treatment assembly 12, macromolecular organic matters in the raw water are removed through the ultraviolet decomposer 121 and the organic adsorber 122 in the water treatment assembly 12, and the raw water is guided to the microsyringe 2 through a pipeline; meanwhile, the water loading unit 3 applies pressure to the water in the flow-through pool 5 through a second injection pump 32 on a water loading pipeline 31, and the water in the flow-through pool 5 is processed through an ion receiver 34 and a heating coil 35 to form water loading which enters the microsyringe 2; the microsyringe 2 mixes the raw water and the carrier water to form a sample to be measured, the sample to be measured is discharged through the connecting pipeline, when the sample to be measured passes through the connecting pipeline, the alkaline reagent and the oxidant combined reagent are injected through the reagent injection device 42, then the reaction is promoted through the first conductivity cell 41 and the mixing coil 43, and then the sample passes through the second conductivity cell 41, and the concentration of the urea is obtained through the conductivity measured by the conductivity cell 41 according to the calculation of a formula.

The device for quantitatively analyzing the trace urea mainly utilizes a flow injection analysis technology and an advanced oxidation technology to quantitatively analyze the concentration of the urea in raw water or produced water, wherein the flow injection analysis technology is used for dispersing a sample solution with a certain volume in a reagent carrier, and because the conditions of the solution in a pipeline, such as residence time, reaction temperature, turbulence intensity and the like, are the same, the reaction is not required to reach an equilibrium state, a working curve of a standard solution can be drawn according to a comparison method, and the concentration of a substance to be measured in the sample solution can be measured. The advanced oxidation technology is characterized by generating hydroxyl free radicals (OH) with strong oxidation capacity, mineralizes organic matters into carbon dioxide, water and other substances, and can effectively oxidize small molecular organic matters, namely urea. Through early advanced oxidation experiments, reagent combinations and reaction conditions for effectively oxidizing urea are found, and a working curve of a standard solution is drawn.

The application provides a trace urea quantitative analysis device, it injects oxidant composite solution into the connecting tube through reagent injection device 42 in, makes the effective and trace urea reaction of hydroxyl free radical that it produced, through the experiment, can accurately measure 20 ~ 1000 PPb's trace urea. And the sample to be measured keeps fluidity in the connecting pipeline, so that the sample to be measured is mentioned to a certain extent, the conditions such as residence time, reaction temperature, turbulence intensity and the like in the pipeline are the same, the repeatability of the measurement result is good, and the precision is high. And the pretreatment device 1, the microsyringe 2, the detection device 4, the water carrying unit 3 and the like are integrated to a high degree.

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications can be made without departing from the scope of the invention.

Claims

1. The utility model provides a trace urea quantitative analysis device, includes preprocessing device (1) and detection device (4), its characterized in that: preprocessing device (1) with be provided with microsyringe (2) between detection device (4), preprocessing device (1) is used for handling macromolecular organic matter, detection device (4) are including connecting tube, reagent injection apparatus (42) and conductivity cell (41), wherein connecting tube one end with microsyringe (2) intercommunication, one end is provided with flow cell (5) in addition for receive the water sample that detects the completion, reagent injection apparatus (42) set up the connecting tube is directional microsyringe (2) one end, conductivity cell (41) set up the connecting tube is directional flow cell (5) one end.

2. The quantitative analysis device for trace urea according to claim 1, characterized in that: preprocessing device (1) includes inlet tube (11), water treatment component (12) and drain pipe (13), inlet tube (11) with water treatment component (12) reach drain pipe (13) communicate the setting respectively, inlet tube (11) are used for right water treatment component (12) carry out raw water and carry, water treatment component (12) are used for getting rid of the macromolecule organic matter in the former aquatic.

3. The quantitative analysis device for trace urea according to claim 2, characterized in that: the micro-sampler (2) is a six-way valve, one of the ports (21) of the micro-sampler (2) is connected with the water carrying unit (3), the rest part of the micro-sampler (2) is connected with the ports (21) of the water treatment component (12), the drain pipe (13) and the detection device (4), the micro-sampler (2) is provided with an annular pipeline (22) for mixing water carried in the water carrying unit (3) with raw water in the pretreatment device (1) and inputting the mixed water into the detection device (4).

4. The quantitative analysis device for trace urea according to claim 3, characterized in that: carry water unit (3) include with carry water pipeline (31) that microsample injector (2) intercommunication set up, carry water pipeline (31) to keep away from microsample injector (2) one end with flow cell (5) are connected and are set up carry water pipeline (31) and be provided with syringe pump, ion receiver (34) and heating coil (35), the syringe pump sets up carry water pipeline (31) to point to microsample injector (2) one end.

5. The quantitative analysis device for trace urea according to claim 4, characterized in that: the number of the conductivity cells (41) is two, and a mixing coil (43) is arranged between the two conductivity cells (41).

6. The quantitative analysis device for trace urea according to claim 5, characterized in that: the water treatment component (12) comprises an ultraviolet decomposer (121) and an organic adsorber (122).