CN112834491A - Ammonia nitrogen analysis device and method - Google Patents

Ammonia nitrogen analysis device and method Download PDF

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Publication number
CN112834491A
CN112834491A CN202011616543.8A CN202011616543A CN112834491A CN 112834491 A CN112834491 A CN 112834491A CN 202011616543 A CN202011616543 A CN 202011616543A CN 112834491 A CN112834491 A CN 112834491A
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China
Prior art keywords
color
ammonia nitrogen
reagent
tube
nitrogen analysis
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CN202011616543.8A
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Inventor
王青青
徐志伟
胡建坤
唐小燕
张侣倛
江荣宝
任中强
姚俊杰
张�杰
方晨霁
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Hangzhou Puyu Technology Development Co Ltd
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Hangzhou Puyu Technology Development Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block

Abstract

The invention provides an ammonia nitrogen analysis device and method, wherein the ammonia nitrogen analysis device comprises a plurality of sample cups; the liquid adding part and the transmission part; the three-dimensional moving mechanical arm carries the liquid adding part and the transmission part to move in three dimensions, and is used for adding a reagent into any sample cup and any developing tube, extracting liquid in the sample cup and adding the liquid into any developing tube; the top of the color development tube is provided with an outer convex part, and the inner wall of the outer convex part is inclined downwards from outside to inside; the transfer member is adapted to move to an upper side of the male part. The invention has the advantages of high analysis efficiency and the like.

Description

Ammonia nitrogen analysis device and method
Technical Field
The invention relates to water quality monitoring, in particular to an ammonia nitrogen analysis device and method.
Background
At present, ammonia nitrogen detection in laboratory water mainly depends on manual work, water samples with turbidity and chromaticity interference need to be pretreated before testing, wherein flocculation and precipitation are a main water sample pretreatment method, and compared with a distillation method, the method is short in time consumption and simple to operate. The defects of manual detection are that when a water sample is more and complicated, filter paper is still required to be used for filtering after flocculation and precipitation of the water sample, the process is slow, the water sample after flocculation treatment cannot be detected in time, ammonia nitrogen in the water sample can escape, and the detection result is low.
In the existing analytical instrument, a single channel is mostly adopted for developing color, and after the color development is finished, the detection is directly carried out or a sample is transferred to a spectrophotometer, and the absorbance is measured at the position of 420mm of wavelength. The technology has the advantages of long time period for testing a large number of samples, low continuous testing efficiency, poor repeatability and larger external interference.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the automatic ammonia nitrogen analysis device with good analysis accuracy and high analysis efficiency.
The purpose of the invention is realized by the following technical scheme:
the ammonia nitrogen analysis device comprises a plurality of sample cups; the ammonia nitrogen analysis device also comprises:
the liquid adding part and the transmission part;
the three-dimensional moving mechanical arm carries the liquid adding part and the transmission part to move three-dimensionally, reagents are respectively added into any sample cup and any color tube by using the liquid adding part, liquid in the sample cup is extracted by using the transmission part, and the liquid is added into any color tube;
the top of the color development pipe is provided with an outer convex part, and the inner wall of the outer convex part inclines downwards from outside to inside; the transfer member is adapted to move to an upper side of the male part.
The invention also aims to provide an ammonia nitrogen analysis method using the ammonia nitrogen analysis device, and the invention aims to be realized by the following technical scheme:
the ammonia nitrogen analysis method using the ammonia nitrogen analysis device comprises the following steps:
(A1) moving the three-dimensional moving mechanical arm, adding a first type of reagent into the selected sample cup by using the liquid adding part, and reacting the sample with the first type of reagent;
(A2) the transmission part extracts the solution in the selected sample cup, the bottom end of the transmission part extends into the outer convex part, and the solution in the transmission part flows downwards along the inner wall of the outer convex part in an inclined way and then flows downwards along the inner wall of the color development pipe;
(A3) the single-shaft mechanical arm moves, a second reagent is added into the selected developing tube by using the liquid adding part, and the solution and the second reagent generate a developing reaction;
while the color development reaction is occurring, adding the solutions in the plurality of sample cups to the other color development tubes by means of the steps (A1) - (A2), and completing the application of the second reagent, and the color development reaction is performed on the parts in the other color development tubes;
(A4) transferring the solution after the color reaction to a detector for detection;
the application, color reaction and detection of the second type reagent in any color developing tube are carried out in sequence and circularly.
Compared with the prior art, the invention has the beneficial effects that:
1. the structure is simple;
the functions of uniformly mixing, filtering, sampling and the like of a high-flux sample can be completed by adopting a transmission part, the sampling needle and the filter screen are integrally formed, the sample residue is reduced, the filter screen can filter particles with the particle size of more than 30 mu m in the sample, and the sampling needle is automatically cleaned;
2. the analysis accuracy is good;
the inner wall of the outer convex part at the upper end of the color development tube is inclined, so that liquid is effectively prevented from splashing and dripping in the quantitative process of the sample, and the quantitative accuracy is improved;
the photoelectric liquid level sensor is arranged, so that the accuracy and stability of sample quantification are improved;
the polyhedron design and the through hole design of the cleaning head improve the cleaning effect of the color developing tube, prevent cross contamination and improve the analysis accuracy;
3. the analysis efficiency is high;
the plurality of color development tubes circularly alternate for color development, and the application and color development of the second reagent are carried out in other color development tubes while color development is carried out, so that the analysis efficiency is remarkably improved, and the color development waiting time is saved;
4. the service life is long;
the merging groove can protect the device when liquid overflows abnormally in the color tube, and the service life of the device is prolonged.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic structural diagram of an ammonia nitrogen analysis device according to an embodiment of the invention;
FIG. 2 is a schematic view of a plurality of color tubes alternately developing colors according to an embodiment of the invention.
Detailed Description
Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a schematic structural diagram of an ammonia nitrogen analysis device according to an embodiment of the present invention, and as shown in fig. 1, the ammonia nitrogen analysis device includes:
a plurality of sample cups, which are prior art in the field;
the liquid adding part and the transmission part;
the three-dimensional moving mechanical arm carries the liquid adding part and the transmission part to move three-dimensionally, reagents are respectively added into any sample cup and any color tube by using the liquid adding part, liquid in the sample cup is extracted by using the transmission part, and the liquid is added into any color tube;
the top of the color development pipe is provided with an outer convex part, and the inner wall of the outer convex part inclines downwards from outside to inside; the transfer member is adapted to move to an upper side of the convex portion so that the liquid output from the transfer member is inclined downward along an inner wall of the convex portion and flows down along an inner wall of the color developing tube;
in order to prevent the liquid in the color developing tube from accidentally escaping to protect the device, the ammonia nitrogen analysis device further comprises:
a receiving groove, wherein the color development pipe is arranged in the receiving groove, and the convex part is positioned at the upper side of the receiving groove; the projection of the color rendering pipe on the water surface completely falls in the projection of the receiving groove on the horizontal plane; the direction of the outward convex part of each color development tube is consistent.
In order to improve analysis efficiency, further, the three-dimensional moving robot arm includes:
the first mechanical arm, the first reagent liquid adding part and the first transmission part are arranged on the first mechanical arm;
the second mechanical arm is provided with a second type reagent feeding part and a second transmission part; the first transmission component and the second transmission component are communicated.
In order to integrate the functions of sampling, filtering and mixing, further, the first transmission part comprises:
a sampling needle disposed on the first robot arm;
a filter member disposed within the sampling needle;
and the pump is arranged on the connecting pipeline between the first transmission part and the second transmission part.
In order to wash the color development pipe, further, the ammonia nitrogen analysis device further comprises:
the cleaning unit, the cleaning unit includes pipeline and shower nozzle, the shower nozzle is the polyhedral structure, and a plurality of through-holes set up on the shower nozzle, the central axis of through-hole and the contained angle between the center axis of shower nozzle are the acute angle.
In order to accurately quantify liquid, the ammonia nitrogen analysis device further comprises photoelectric liquid level sensors which are arranged on two sides outside the color developing tube.
The ammonia nitrogen analysis method of the embodiment of the present invention, that is, the operating method of the ammonia nitrogen analysis apparatus of the embodiment of the present invention, includes the following steps:
(A1) moving the three-dimensional moving mechanical arm, adding a first type of reagent into the selected sample cup by using the liquid adding part, and reacting the sample with the first type of reagent;
(A2) the transmission part extracts the solution in the selected sample cup, and the solution in the transmission part flows downwards along the inner wall of the outer convex part in an inclined way and then flows downwards along the inner wall of the color development pipe;
(A3) the three-dimensional moving mechanical arm moves, a second reagent is added into the selected developing tube by using the liquid adding part, and the solution and the second reagent generate a developing reaction;
while the color development reaction is occurring, adding the solutions in the plurality of sample cups to the other color development tubes by means of the steps (A1) - (A2), and completing the application of the second reagent, and the color development reaction is performed on the parts in the other color development tubes;
(A4) transferring the solution after the color reaction to a detector for detection;
the application, color reaction and detection of the second type reagent in any color developing tube are carried out in sequence and circularly.
To improve the efficiency of the assay, further, the time of application of the second type of reagent is determined for each cyclet1And at the time of detectionWorkshopt2Sum of
Figure BDA0002876874220000051
t3In order to achieve the color reaction time,Nthe number of the color developing tubes.
In order to improve the analysis efficiency, in any color development reaction time in the color development tube, the detection of the previous cycle corresponding to other color development tubes and the application of the second type reagent of the next cycle are simultaneously carried out, and the application time of the second type reagent of the color development tube corresponding to the previous detection is set in the time between the adjacent two detections of different color development tubes corresponding to the detectors.
In order to improve the analysis efficiency, when the detection corresponding to any one of the color tubes is started, the color reaction in the other partial color tube is started, and the color reaction in the partial color tube is in progress.
Example 2:
the ammonia nitrogen analysis device and the method provided by the embodiment 1 of the invention are applied to the application example.
In the application example, a plurality of sample cups are arranged in a matrix form, three color development tubes are arranged in a straight line, and the direction of the convex parts is consistent;
the three-dimensional moving mechanical arm comprises a first mechanical arm and a second mechanical arm, and the liquid adding part comprises a first liquid adding part, a second liquid adding part, a third liquid adding part and a fourth liquid adding part; the openings of the first liquid adding part and the second liquid adding part are downward and are arranged on the first mechanical arm; the openings of the third liquid adding part and the fourth liquid adding part are downward and are arranged on the second mechanical arm; each liquid adding component comprises a quantitative module and a pipeline, and a quantitative reagent passes through the pipeline to enter the sample quilt or the color tube;
the transmission component comprises a first transmission component and a second transmission component, the first transmission component comprises a sampling needle, a filtering component and a pump, the filtering component is arranged in the sampling needle and is integrally formed, and the sampling needle is downward in opening and is arranged on the first mechanical arm; the second transmission component comprises a sample adding needle; the pump is arranged on a pipeline for communicating the sampling needle and the sample adding needle;
the color development tube is arranged in the receiving groove, and the convex part is positioned on the upper side of the receiving groove; the projection of the color rendering pipe on the water surface completely falls in the projection of the receiving groove on the horizontal plane; the orientation of the external convex part of each color development tube is consistent; a three-way valve is arranged at the lower side of each color development pipe, liquid in the color development pipe is discharged to the downstream through the three-way valve according to requirements, and air enters the color development pipe through the three-way valve;
the cleaning unit comprises a pipeline and a spray head, the spray head is in a polyhedral structure, a plurality of through holes are formed in the spray head, and an included angle between the central axis of each through hole and the central axis of the spray head is an acute angle; the spray head is arranged on the second mechanical arm;
the photoelectric liquid level sensors are arranged on two sides outside the color developing tube.
The ammonia nitrogen analysis method of the embodiment of the present invention, that is, the operating method of the ammonia nitrogen analysis apparatus of the embodiment of the present invention, includes the following steps:
(A1) the first mechanical arm moves, a first liquid adding part is utilized to add a first reagent, namely sodium hydroxide, into the selected sample cup, and a second liquid adding part is utilized to add a first reagent, namely zinc sulfate, into the selected sample cup;
the sampling needle descends and enters the liquid level, air is input by the pump, the air enters the liquid from the sampling needle, so that the liquid and the first reagent are mixed, and the sample reacts with the first reagent;
closing the pump, and standing to complete flocculation and precipitation;
(A2) the second mechanical arm moves to the upper side of the selected first color rendering pipe,
the sampling needle extends into the liquid level of the sample cup, and liquid after reaction is extracted under the action of a pump; the solution flowing out of the bottom end of the sample adding needle flows downwards along the inner wall of the outer convex part in an inclined mode and then flows downwards along the inner wall of the first color development tube;
(A3) the second mechanical arm moves, and a second reagent, namely a potassium sodium tartrate solution is added into the selected first color tube by using a third liquid adding part; opening a valve at the lower side of the first color development tube, enabling air to pass through the valve and enter the first color development tube, thereby uniformly mixing the sample, and closing the valve;
adding a second reagent, namely a nano reagent, into the selected first color developing tube by using a fourth liquid adding part; opening a valve at the lower side of the first color development tube, enabling air to pass through the valve and enter the first color development tube, thereby uniformly mixing the sample, and closing the valve;
as shown in fig. 2, the sample is allowed to stand in the first color developing tube for color development; while the color reaction is occurring, sequentially adding the solutions in the plurality of sample cups to the second and third color tubes in the manner of steps (A1) - (A2), wherein when the color reaction in the first color tube is finished, the application of the second reagent in the second color tube is finished, and the application of the second reagent in the third color tube is finished while the color reaction is in progress;
(A4) transferring the solution after the color reaction to a detector for detection;
in the process, the application, the color reaction and the detection of the second reagent in any color developing tube are sequentially and circularly carried out; the time of application of the second type of reagent in each cycle of the respective developing tubet1And the time of detectiont2Sum of
Figure BDA0002876874220000071
t3In order to achieve the color reaction time,Nthe number of color developing tubes in this embodimentN=3
In the color development reaction time in any color development tube, simultaneously carrying out the detection of the last cycle and the application of the second type of reagent of the next cycle corresponding to other color development tubes, wherein the application time of the second type of reagent of the color development tube corresponding to the prior detection is the time between the adjacent two detections of different color development tubes corresponding to the detector; when the detection corresponding to any color developing tube (such as the first color developing tube) is started, the color developing reaction in other part of the color developing tubes (third color developing tubes) is started, and the color developing reaction in part of the color developing tubes (second color developing tubes) is in the process of proceeding;
when the inner wall of the color developing tube is cleaned, the second mechanical arm drives the cleaning agent to penetrate through the pipeline and discharge from the through hole of the cleaning head, and the color developing tube is cleaned.
Example 3:
the application example of the ammonia nitrogen analysis device and method according to the embodiment 1 of the invention is different from the embodiment 2 in that:
1. only one three-dimensional moving mechanical arm is provided, a plurality of liquid adding components are arranged on the mechanical arm, and the transmission component only comprises a sample adding needle, a pump and a pipeline; through three-dimensional removal arm for the liquid in the application of sample needle extraction sample cup and keep in, treat application of sample needle and when the arm moved the convex part in the color rendering pipe of selection in along with the arm, discharge the liquid of keeping in.
2. The number of the color development tubes is two.

Claims (10)

1. The ammonia nitrogen analysis device comprises a plurality of sample cups; it is characterized in that the ammonia nitrogen analysis device further comprises:
the liquid adding part and the transmission part;
the three-dimensional moving mechanical arm carries the liquid adding part and the transmission part to move three-dimensionally, reagents are respectively added into any sample cup and any color tube by using the liquid adding part, liquid in the sample cup is extracted by using the transmission part, and the liquid is added into any color tube;
the top of the color development pipe is provided with an outer convex part, and the inner wall of the outer convex part inclines downwards from outside to inside; the transfer member is adapted to move to an upper side of the male part.
2. The ammonia nitrogen analysis device of claim 1, further comprising:
a receiving groove, wherein the color development pipe is arranged in the receiving groove, and the convex part is positioned at the upper side of the receiving groove; the projection of the color rendering pipe on the water surface completely falls in the projection of the receiving groove on the horizontal plane; the direction of the outward convex part of each color development tube is consistent.
3. The ammonia nitrogen analysis device according to claim 1, wherein the three-dimensional moving mechanical arm comprises:
the first mechanical arm, the first reagent liquid adding part and the first transmission part are arranged on the first mechanical arm;
the second mechanical arm is provided with a second type reagent feeding part and a second transmission part; the first transmission component and the second transmission component are communicated.
4. The ammonia nitrogen analysis device of claim 3, wherein the first transmission part comprises:
a sampling needle disposed on the first robot arm;
a filter member disposed within the sampling needle
And the pump is arranged on the connecting pipeline between the first transmission part and the second transmission part.
5. The ammonia nitrogen analysis device of claim 1, further comprising:
the cleaning unit, the cleaning unit includes pipeline and shower nozzle, the shower nozzle is the polyhedral structure, and a plurality of through-holes set up on the shower nozzle, the central axis of through-hole and the contained angle between the center axis of shower nozzle are the acute angle.
6. The ammonia nitrogen analysis device of claim 1, further comprising photoelectric liquid level sensors disposed on both sides of the color tube.
7. An ammonia nitrogen analysis method using the ammonia nitrogen analysis device of any one of claims 1 to 6, comprising the steps of:
(A1) moving the three-dimensional moving mechanical arm, adding a first type of reagent into the selected sample cup by using the liquid adding part, and reacting the sample with the first type of reagent;
(A2) the transmission part extracts the solution in the selected sample cup, and the solution in the transmission part flows downwards along the inner wall of the outer convex part in an inclined way and then flows downwards along the inner wall of the color development pipe;
(A3) the single-shaft mechanical arm moves, a second reagent is added into the selected developing tube by using the liquid adding part, and the solution and the second reagent generate a developing reaction;
while the color development reaction is occurring, adding the solutions in the plurality of sample cups to the other color development tubes by means of the steps (A1) - (A2), and completing the application of the second reagent, and the color development reaction is performed on the parts in the other color development tubes;
(A4) transferring the solution after the color reaction to a detector for detection;
the application, color reaction and detection of the second type reagent in any color developing tube are carried out in sequence and circularly.
8. Ammonia nitrogen analysis method according to claim 7, characterized in that the second reagent is applied for a time t in each cycle1And a detection time t2Sum of
Figure FDA0002876874210000021
t3For the color reaction time, N is the number of color tubes.
9. The ammonia nitrogen analysis method according to claim 8, wherein the detection of the previous cycle and the application of the second reagent of the next cycle corresponding to other color tubes are performed simultaneously within the color reaction time in any color tube, and the application time of the second reagent of the color tube corresponding to the previous detection is within the time between the detection of the adjacent two different color tubes corresponding to the detector.
10. The method for analyzing ammonia nitrogen according to claim 9, wherein when the detection corresponding to any one of the color tubes is started, the color reaction in the other part of the color tubes is started, and the color reaction in the part of the color tubes is in progress.
CN202011616543.8A 2020-12-31 2020-12-31 Ammonia nitrogen analysis device and method Pending CN112834491A (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
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CN111044742A (en) * 2020-01-06 2020-04-21 无锡集佳智能科技有限公司 Intelligent sample processing and detecting device

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN203981575U (en) * 2014-08-14 2014-12-03 河北中检之星仪器仪表有限公司 A kind of full-automatic ammonia nitrogen detector
WO2019154348A1 (en) * 2018-02-11 2019-08-15 北京科美生物技术有限公司 Fully automatic photoexcited chemiluminescence detector
CN110161258A (en) * 2018-02-11 2019-08-23 博阳生物科技(上海)有限公司 A kind of full-automatic light-induced chemiluminescent detector
CN111044742A (en) * 2020-01-06 2020-04-21 无锡集佳智能科技有限公司 Intelligent sample processing and detecting device

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